Nevermind
Time eased my soul for me.

I was just impatient and wanted to know before I could see for myself i guess

Hey everybody, long time reader, first time poster. I just wanted to post and say that my friend just put her last collection jar in the freezer and is extremely excited to see her results. This is her first attempt at doing an extraction of any kind, and after being excited about doing so for five or six years it is awesome to finally see her doing it. She used 200g MHRB and did the extraction following Noman's tek to the T. It was pretty messy, and next time she thinks she will using a gallon pickle jar instead of a jar with a pressure top. She says finding the supplies was a piece of cake between Lowe's and Ace hardware, and she also found perfect 250ml small pyrex dishes with lids at Wal-Mart for very cheap. Wish her luck!

luck

My friend decided to do another extraction after waking up this morning to find her collection jars covered in small white pellets which she believes to be the good stuff. She is wondering if there is a trick to getting the very last tiny bit of naptha off the top layer, or if it is okay to suck it into the turkey baster with a little bit of the basic solution, let the black sing to the bottom of the baster, squeeze it out, then collect the naptha left over in the baster. Will this taint the final product with NaOH? She would like to avoid the ammonia wash, but she will probably recrystalize.

SWIM advises against picking up the black solution... best is to add some more naphta and suck it up again.. If this is your first pull, then you definitely have to do at least another 2 more pulls.. but if this is your last pull, then either you just suck it up as much as you can and leave the last bit since it will be so little spice.. or, what SWIM does (but only if your container is big enough for a glass to fit through the top) is to submerge a glass in the liquid.. as if you are filling up a glass in the pool by putting it under water with the top straight... so what will happen is, as you slowly put it under water, it will first ´suck up´ the top layer, where the naphta is, and then after all that layer is sucked up it will start getting the black liquid.. now you can pull the glass up, and since a glass is thiner, this means the layer of naphta will be thicker, which means it will be easier to separate using pipete/turkey baster..

hope it helps

Okay, SWIM feel likes her extraction is going really well for a first time. After six naptha pulls, she has got one gram of slightly yellowish tiny crystals from 200g MH inner rootbark. She has one problem though, when she attempted to do recrystalization, she had to do it with naptha, since it seems that heptane isn't readily available in her area. She followed the instructions in noman's tek exactly, but after slowly cooling the liquid to room temp, putting it in the fridge, then in the freeze, all she has is the same one gram of slightly yellowish crystals. Basically, the same exact thing that happened in the original six freeze preciptations happened when she tried to recrystalize her product. SWIM is a little bit worried about just trying to smoke the slightly yellow stuff, since she is worried it might have a small bit of NaOH in it, but she is clueless as to why her recrystalization step did not work. She is suspecting that not using heptane is main reason, but input from someone more experienced would be helpful. At this point she has read a lot of horror stories about ammonia washing, although she does have 10% janitorial strength ammonia from ace hardware.

I often get the same kiknd of thing happening when I try and use naphtha for the recrystlization, you might wanna try looking into doing a baking soda wash..

Check out the post by acolon here:
http://www.dmt-nexus.me/....aspx?g=posts&t=1408

I dont think its about using naphta because SWIM only uses naphta and recrystalization works perfectly

When SWIY dissolved the crystals back into naphta, was there some oily dark orange/red/brown layer on the bottom? there should be something like that and SWIY should separate the naphta from it...

What SWIM does is put the crystals in a shot glass, boil some water, turn off the fire, put 30ml of naphta per g of crystals in the shot glass, then sink the shot glass´ bottom in the water and make swirling movements to help dissolving the crystals.. then in a minute or so the crystals should dissolve and this oily dark layer remain... then SWIM just pulls all the naphta he can with pipette, and the last little bit, where he is not ´accurate´ enough to suck, he adds like 5ml more of naphta, swirls a bit more and remove all he can of naphta and puts together with the rest.. if there is a tiny bit left together with the crude layer its no problem... then stick in the fridge and should def be lighter colour/cleaner

another thing SWIY can do to remove any traces of NaOH is to do not an ammonia wash (many ppl have problems with it) but instead do a sodium carbonate (washing soda.. also sold as ´pH up´, a product sold for increasing the pH of pools)... I recommend against baking soda (sodium BIcarbonate) too..

so what you do is basically just make a pH 9 adjusted water (a tiny tiny tiny pinch of sodium carbonate in, like, 50ml of water), and put that in a small water bottle or smt.. then put the naphta with the dmt dissolved in it in the bottle too, shake like hell (dont worry no emulsions form).. then separate the layers, and put another 50ml of just pure water, mix again, separate, and thats it, now you can be sure no NaOH traces

SWIM did some searching and got sodium carbonate and did that wash process. SWIM thinks she could see the residual lye impurities rolling around the bottom of the jar of naptha she used. She added quite a bit of naptha, finally getting everything to dissolve except for a little clump of yellow stuff that stayed right on the bottom even with a lot of shaking. When she tiled or rolled the jar, the clump all stayed together and rolled around in the bottom of the jar. When she added her sodium carbonate solution, the clump disappeared, which seems like a good sign. She tried smoking some of the pre-wash spice, and it was extremely harsh. It left an oily residue in her pipe also. SWIM doesn't think she smoked enough to get a breakthrough experience even with very good product, but just wanted to test how harsh the smoke was and what it left behind. She did feel some effects, but they were overwhelemed by the burning throat.

A wash should help fix that problem. Just remember to do the wash on the naphtha not the actual crystals or you will only be washing a very small fraction of the spice.

Hi all,
I heard about someone doing a MMHR extraction who after getting the spice into the solvent set a jar of it out in the sun with a paper towel covering the top with a rubber band. After a few hours the solvent got cloudy white and there was a lot of stuff that had solidified out into the solvent that looked like spice. He capped and put the solvent back into the freezer and then the stuff all disappeared again leaving a small amount of brown trash on the bottom of the jar. Has anyone had any experiences like this. The solvent/spice looked very clear initially. He did have a little emulsion that had carried over after doing a washing soda/water wash. Initially upon freezing there were a few crystals that had precipitated but there hadn't been a heavy reduction in volume done.

I advised this person that next time he tries it he should filter the stuff out of the solvent. Either way it would be a good thing to do. If it's trash it would clean up the mix if it is spice he could clean that up and keep it.

That person really needed to get all of the wash water out. Better to loose a few mL's of naphtha than have extra impurities in the spice.

Filter, reduce volume, make sure all the wash is out, and freeze!

Greetings to all, and thank you for allowing me on the forum.

Having read to most of the teks available here and elsewhere, and having an analytical mind, I have some questions. Now, I understand that extracting the Spice is more of an art than a exact science, but I am inclined to approach it as a set of lab-instructions. So here goes:

A) In using a blender to grind up your MHRB, why not add the pH4 water to the material in the blender and then blend it? Wouldn’t the added bonus of the strong mechanical blending together of solvent (water) and material weigh up to the downside the water slowing down the blades somewhat? Dust would also be eliminated. Any metals dissolving from the blades may be an issue, but they would certainly precipitate out in the alkaline step (hardly any soluble metal-hydroxides exist), and pH4 isn’t very acidic to begin with: I suppose most fruit blends are more acidic than that.

B) Why does Vovin’s A/B tek and others use lye in such low concentrations? Using pH13 water to make pH4 water pH12 is not very economical. My chemists’ mind tells me to use a 30% solution, or a buffer. Like this, the need for a reduction step would almost certainly be eliminated. As the strong lye is added, would the brief extremely alkaline environment be detrimental to the transition of DMT salt to DMT base?

C) To boil or not to boil? Some teks boil the MHRB in water, others just infuse it at warm temperatures. I know that the traditional Ayahuasca recipes boil their mixture vigorously. I also know that DMT.HCl is not exactly unstable, but only to a certain degree (pun intended). Why the heating? To break up tissues and reduce volume at the cost of DMT?

D) I haven’t read of MEK (2-Butanone) or Freon being used. In my experience MEK is an awesome liquid/liquid extraction solvent, forming emulsions only with the most strong of emulsifiers. If this hold out for MHRB-soup, one could give it a really good shake. Freon is bad for the planet and very difficult to come by, but quite inert at room temperatures. Would they extract Jungle Spice as well? Any thoughts on these?

E) There is a formula for calculating the most efficient number of volumes to use in a liquid/liquid extraction (like in 2x50ml or 4x25ml). Unfortunatly, one needs the (how’s that in English) Kv or Coefficient of dispersion for that. Has anyone experimented for it in MHRB-water or does anyone know it for DMT?

I’d love to have some feedback on these!

Peace.

Blending in acidified water creates massive bubbles that take forever to go down. Try it and see! If using vinegar I wouldn't be worried about leaching metals, but if using HCL it would be a problem (probably with phosphoric acid as well).





Some people put NaOH directly into the stew, but I have read that the pH spikes caused by this (not to mention the heat created) destroy some of the spice. Hence, the need to have it in solution first. If doing an A/B there really is no need to bring it up to much past 11.5-12.0 and it does not take much lye to achieve this from ph 3 or 4.



Never had a problem using heat. It speeds up the extraction process from weeks to hours. Try doing a cold A/B extraction. You will find that unless you soak for days to weeks, you will have a very, very small yeild.



Can't freeze precipiate from MEK. Freeze precipiation is one of the best ways us kitchen chemists purify our product. It is better (and quicker) for us to have to do 4-5 NP solvent pulls and stick them in the freezer than wait for evap. It also results in a much cleaner product.



Not a clue.

The methods you see around have been tried and true. If you can create a new tek or improve on an existing one, I am all ears!

Thanks for the input. Its all sound advise, and I'll take it to heart. Except for the lye. I'll make a somewhat stronger lye solution than vovin's tek describes: like 2M (Noman's tek uses 1.5M). I'll do a grid of variable extractions in the future to get an approximation of the Kv.
Thanks again.

agree with the former, swib found it takes a considerable amount of base,(extracting with vinegar..at least double the volume with 2M) to get it past the buffer range (around pH4 - 7)

swib is gonna try a soxhlet extraction next,with 85EtOH/15MeOH, and then do A/B on the residue... or just freeze it to see if it crashes out.

This site allows one to calculate the pH of single solutions or mixtures easily. I've rounded the numbers a bit.

The acidic soup should be pH 3-4, meaning that for 500 ml of soup as his tek describes, it should have about 0.5g of HCl in it(mind you, the v is not necessary for single solutions:
HCl pKa=-7 v=500 c=0.001 (HCl in concentrated form is about 33% pure, triple the mole weight(36.5*0.001) for a 0.001M solution, or 1g for a liter, or 0.5g for half a liter
[H+] = 0.001
pH = 3.000

What does Vovin's tek describe? pH of his basifying solution is 12-13, which is about 0.1M:
NaOH pKb=-0.2 v=500 c=0.1
[OH-] = 0.0944
pH = 12.975

So, he dissolves 2g of NaOH (mole weight 40) in 500 ml. Now we combine the two:
NaOH pKb=-0.2 v=500 c=0.1
HCl pKa=-7 v=500 c=0.001
[H+] = 2.082E-13
[OH-] = 0.04803
pH = 12.68
pOH = 1.32

Indeed, the pH we're aiming for. But I want a stronger lye, let's say 10ml of 2M solution, or 8g in 100ml, or 0.8g in 10ml:
NaOH pKb=-0.2 v=10 c=2
HCl pKa=-7 v=500 c=0.001
[H+] = 2.679E-13
[OH-] = 0.0373
pH = 12.572
pOH = 1.428

Which is over pH12. Using double the amount of 2M lye nets your pH12.86 which is still good, me thinks.
One just has to make sure to add the 10ml dropwise with good swirling, to minimize excessive concentrations locally.
However, this all just purely theorical: perhaps the solution has buffering qualities; I don't know.
The salts also eat away at some of the free [OH-], perhaps half a mole for 0.5g of DMT in the solution, a little more if other components are in the mixture. So, add about half a mole extra, or 25% more solution.

I think SWIM can experiment with this.
I agree the tried and tested methods are safer, but hey! I like a little experimentation.

Peace.

PS: I just realized Vovins tek describes the reducing of the soup from 1L to half a liter before the basifying step. Using HCl, which forms an azeotrope with water, the pH of the soup would be lower still.

Hey


I was reading up on a pretty simple technique (http://forums.mycotopia.net/holding-tank/34478-clean-easy-stb.html)

and it does everything at room temperature which is different from most of the other techniques i have seen

so my question is

does the naphtha absorb the spice when it isn't hot?



thanks

[For the chem gurus]

When putting the spice in the freezer for crystallization would it be a better idea to first freeze the final solution in liquid nitrogen before putting it in the deep-freezer?