Procedure D - Reduction and freebasing (hot and spicy)
It’s been suggested that DMT-n-oxide also reacts with fumaric acid to form fumarates. Hence, there should be some in my
total fums. I am hoping to convert this to DMT, proven by higher yields as compared to
procedure C for sure (because I de-fatted and filtered that one), and to
procedure B perhaps (because the oxide should also crash out in that one, and the presence of those yellow blobs in there would suggest that they might have). What’s more, I secretly hope that the ‘chunks’ I got on the bottom of the beaker with
pool 1 and
pool 2 were oxides. If so, I should really have a higher yield as with
B and
C, assuming the reduction with zinc works at all.
At first I wanted to see if different types of acid would change the outcome, but decided against it. There are a few experiments with hydrochloric described here on the Nexus, but they didn’t seem to work that good. I’ve also read here that all the successful experiments as carried out by researchers years ago were all done with acetic acid. I didn’t read those papers, so I decided to make the concentration the variable. I prepared some 36% from glacial, and used it to make various strengths: 9% (table-vinegar), 18% (pickling-vinegar) and undiluted 36% (un-culinary strength!) concentrations. That last one seems concentrated enough to me: I’ll forego on using glacial neat. The zinc used was obtained from a chemical company, and was ultra-fine. Literally as fine as could be, but sorry: no BET-value available.
9% acetic acid - method, observations, musings
1.00 g of the
total fums was dissolved in a 100 ml beaker in 45 ml water and 15 ml of 36% acetic acid was added to this, making it a 9% vinegar-solution. The colour was PMS 101 and it was slightly murky. 2 g of Zn powder was added and the contents of the beaker immediately stirred vigorously to get a suspension of Zn for as long as it would stay buoyant. Which was about 5 minutes, and the solution was totally clear and colourless when the zinc had sunk. A few bubbles of presumably hydrogen came into being at the zinc’s surface, making the whole reaction just slightly effervescent. I hoped that the bubbles emanating from the centre of the beaker would create some kind of convection in there, assuring a circulating flow of all reducible material to the source of nascent hydrogen. The zinc-powder would coalesce into blobs, presumably by the difference in surface-tension between the vinegar and the bubbles of hydrogen. All this was left to stand for 4 hours with a quick stir every hour or so. The pH of the solution was 4 in the end (test-paper). I wonder if this could be correct; I calculated it to be around 2. Could the fumarates and Zn have used up so much protons? My pH paper is old though, it could be off a bit and so could my interpreting the papers’ colours.
After these 4 hours, I filtered the solution (recovered 1.8 g of Zn), washed the filter with 3 x 20 ml of fresh water and transferred everything to my trusty Coulter-glass. I did have to add a
lot of saturated Na2CO3 solution before it was all even neutral. This does not bode well for the 18 and 36% solutions; I can’t add a quadruple amount! So for the 18% I will have to make a super-saturated solution using 60+ centigrade water, and for the 36% I will neutralize to pH 4 with NaOH solution first. This is an important side-effect of using crash-out purification to freebase in this way. Extracting with naphtha (to really liberate it from the basic solution) would be better , but I just don’t want to skew the numbers right now (I could have unforeseeable losses from handling such small amounts). Adding the carbonate-solution generated a lot of gas. I stopped basifying when the precipitate persisted. It measured pH 8. I put the beaker of now totally white (and I mean white!) milk to rest for the night. Wut??? No crystallizing observable, just a bottom of milky sludge. Ok then: extracting. Extracted with 4 x 25 ml of naphtha. The white muck remained in the polar phase all the time. I conclude it is Zn(OH)2, as zinc is the only anion apart from hydrogen that I can imagine being in there. Most metal-hydroxides are insoluble in water. This also means my elaborate plans for basifying the next two acetic acid solutions can be tossed out: if I’m going to extract anyway I might as well use any amount of NaOH needed.
After the extraction, I extracted once more with 15 ml of naphtha and let this evaporate quickly on a warm glass dish. Something translucent stayed behind in the dish, but it was close to nothing, and it also did not smell like DMT very much when heated. After heating it left a nasty stain on my spatula, so it’s probably some hydroxides that carried over (I didn’t dry this test-fraction). 100 ml of naphtha should hold 1 g of DMT. I have a theoretical 0.76 g in there, so I should have 95% of the spice in the naphtha now. I dried the main naphtha extract by filtering through some anhydrous Na2SO4 and washing the filter with 2 x 10 ml of fresh naphtha, I popped the naphtha (it was 110 ml) in the freezer for 48 hours. BTW: all my naphtha in all these “acetic acid/total fums” procedures was always completely colourless. Not even a hint of yellow. After decanting the naphtha and drying the goodies, I got 0.39 g of totally white, sparkly goodies. (see pic, Holy depth of field Batman! Oh: sorry about the red lint. The yellow tan is due to some radiosity effect from my putting the lens at an inch’s distance from the stuff)
I wasn’t pleased with that amount, so I increased the pH of the solution to 12 and re-extracted with the same naphtha (3 x 30 ml). I tell you, extracting this much more basic solution was a pain. I got a lot more emulsions and separating was more troublesome. The Zn(OH)2 stuck to every bit of glass it came into contact with, especially my separating-funnel.
After 16 hours in the freezer (so short because my naphtha should already be saturated with DMT at the temperature I freeze-precipitate) quite a few more crystals crashed out. These were removed like above and they looked like above. They weighed in at 0.15 g, for a total of 0.44 g of very white, and I assume pure, DMT. That’s 44% based on the salt, or a yield of 57% of theoretical. This is less than my de-fatted
procedure C spice. Darn! That’s bad. On the other hand, this stuff is SO white, it’s impressive. It’s possible that increasing the concentration of the acetic acid will increase the yield.
Incidentally, I assessed these two DMT’s separately:
9% - qualitative
pH 8 spice:
Bodymind: Oh my… SO intense, deep and fast... SO completely techno and yet with some very extreme interludes of something completely different, like a window or porthole opening to a completely other space, for split-seconds at a time…. But all the while so completely impersonal. I felt nothing: no empathy, no apprehension, no friendliness, no love, no hate, no nuthin’. And the bodily residual feeling started so early, like halfway through, and it was so stoning. I felt as if I sank a foot into the leather recliner I was sitting in. I yawned and yawned (physical reaction to whatever) until my jaw felt sore and I just *had* to force my body from the chair.
Entities: None. There was nothing and nobody.
Taste/appearance: Excellent taste! Loved every bit of this! And for the looks: well, the white spice always looks nice. This one is a bit more… like lemon sherbet. You know, opaque white instead of clear.
Verdict: This felt like a souped-up version of
pool 2 JJS but more impersonal and with the residues feeling twice as stoning. It was more easy to snap out of them though… For me, this experience was precisely what I was trying to get away from, bar the absence of gems in my mouth. Perhaps at a higher dose it could still be worthwhile, but at this level: no. Finding out if this higher-dose paradigm hold true for me will mean experimenting on myself and that is beyond the scope of this report.
pH 12 spice:
Bodymind: Pretty much the same as the pH8-DMT, but feeling more benign. Everything felt more ‘stretched’, including having CEV’s whilst deep in the residual phase. It could be I have smoked less efficient this time.
Entities: Same as before
Taste/appearance: Same as before. The purple colour in the photograph is because I had switched on my space-lights in the room. Sorry about that, but it does look nice, no?
Verdict: My opinion is the same as with the pH 8 spice. I will combine the two spices. They feel and look completely interchangeable.
The thought of trying to transform this spice back into ANY
procedure C DMT keeps crossing my mind. It would entail giving it back to my perfumed spice, FASA-salting it and freebasing again. Then again, it could be an excellent candidate for trying my hands on some re-crystallization with heptane….
18% acetic acid - method, observations, musings
Dissolved 1.00 g of
total fums in 30 ml of water, added 30 ml of 36% acetic acid (pH=3) and added 2.0 g of powdered zinc. Everything went as before, except for the slightly more frothy reaction and an unspeakable, faecal smell (and I don’t mean it smelled like shit, it just smelled like, well, shit.)
After four hours, I lost 350 mg of mass and I recovered 1.80 g of zinc, again (huh?)
Basifying until neutrality used up quite a lot of 10% NaOH. It’s easy to see, because the precipitate of Zn(OH)2 becomes persistent whereas before it re-dissolved in the solution. A dash of extra lye immediately pushes it to pH12, releasing the tell-tale smell of tryptamines into the air. (yum!)
Extracting was a bitch this time. ALL the hydroxides were afloat, and mixed themselves with the naphtha.
I had to treat this “hydroxide” layer separately in a beaker and saturate it with a dozen or so teaspoons of Na2CO3. This had a threefold effect: it bound to the water and made it sink to the bottom taking some hydroxides with it, it reduced the ratio of hydroxides to water, and because this reaction is exothermic it facilitated the separation of the naphtha even more. So, no biggie but still a hassle compared to the previous (9%) experiment. I also resorted to gently rocking the funnel for five minutes, as opposed to my usual “shaking the hell out of it for 20 seconds”. Repeated this several times, pooling the solvents in a 100 ml separating funnel. The clear watery, hydroxide-free phase was also extracted 3 times and the solvent added to the funnel for final separation and washing with fresh water. Incidentally, I re-used all the naphtha from the freeze precipitation of the previous experiment (plus some extra). I know it will slightly skew the results (again), but I choose to be efficient wilfully.
I used a lot more naphtha this time (6 x 25 ml) so I let it evaporate overnight to about half that, then dried over sodium sulphate and popped it into the freezer for 24 hours.
I took the crystals out as before and dried. It yielded 0.35 g of the exact same spice, from an appearance point-of-view. That’s 35% based on the salt, or a yield of 46% of theoretical. So little…. These yields go down and down, most likely because of all the extra steps, washings and extractions involved. The percentile losses just keep piling up, resulting in less and less freebase, and so far less and less qualitatively desirable freebase at that, too...
18% - qualitative
It all feels the same as both the 9% DMT’s.
36% acetic acid - method, observations, musings
Dissolved 1.00 g of
total fums in 60 ml of 36% acetic acid (pH=2, no really. Doubling the concentration does indeed decrease the pH by 1 point each time. Note that you’ll never reach pH 0 with this.) and added 2.0 g of powdered zinc. Reaction proceeded as before, this time with an even stronger bubbling. I can still hardly describe it as ‘vigorous’ though. I lost 1 gram of mass in the reaction, and 1.5 g of zinc was recovered. If I was to remove any unwanted non-polar components, this would be the time to extract them. Extracting with 2 x 20 ml naphtha while the solution is acidic is the way to go here.
Wizened from the previous experience, I basified to pH8 using a lot of 20% NaOH (3 times as much as there was solution, for a total volume of about 200 ml!) and extracted with 3 x 20 ml of the naphtha that was recovered from the previous freeze precipitation. The solution became quite hot during basification. After these 3 pulls, the polar phase was basified to pH12 (it needed just 10-20 ml more lye-solution) and extracted again with 3 x 20 ml naphtha. I like the results of this 2-step extraction: it makes dealing with the hydroxides a lot less troublesome. The pooled extracts were dried over Na2SO4, left to stand overnight to evaporate to about 90 ml (yes, that’s the reverse of what I did before) and put into the freezer in the morning. 36 hours later, they were removed and separated from the naphtha as before. The crystals weighed in at 0.58 g! That’s 58% based on the salt, or a yield of 76% of theoretical. Finally, I got more than my
procedure C spice and even more than
procedure B. This is more like it. I see this as a strong indication that there is something being turned from non-DMT into DMT proper. Whether the product of this reduction is desirable however, is a matter of personal preference. It’s too bad I did not follow the exact same procedure with all three reductions to make the comparison really solid. For instance, it might be that not all DMT had precipitated in previous freezes and the surplus was deposited out of the recycled naphtha with this freeze, giving rise to the following: 0.44 + 0.35 + 0.58 = 1.47 g of combined DMT from 3.0 g of
total fums, a 49% yield based on the salt, or 64% of theoretical. The yield, on average, being so low could mean that either Zn-reduction doesn’t work or, more hopeful, that hardly any reducible material was present in the
total fums. This would mean that DMT-n-oxide had NOT precipitated with FASA-salting, and that the 31% I was missing at
procedure B, whatever it is composed of, cannot be converted into DMT. Yet the data is sketchy and a reduction of the
JJS should give more conclusive evidence. But I do have enough data now to postulate a guideline:
• Use no less than 36% acetic acid. 72%
might be best. 100% is probably too much.
• Use at least equal the mass of zinc to the mass of spice.
• Let the reaction proceed for at least 4 hours.
• Use two-step basifying and extracting with 10% NaOH-solution at pH8 and subsequently pH12. If nothing else, it will make extracting the freebase so much more easy and reduce losses.
• Extract 3 times at both pH-levels, using a volume of 20 times the weight of spice for each.
• Evaporate to a volume of 100 times the weight of spice used. Evaporating to 50 times is better.
• Let pooled extracts freeze for at least 36 hours.
• Collect snow-white DMT (shut up, Dopey. GTFO!).
BTW: I evaporated the naphtha after it gave up all of it’s DMT in all freezes. It yielded no more than 20 mg of DMT, from about 90 ml. Sweet!
36% - qualitative
Again, this spice feels the same as the other three kinds above. Between all of them, there were subtle and sometimes less subtle differences, but I attribute those to changes in my smoking efficiency, as well as my bodily state and mental state at those times. The visuals all sing to the same tune (very laser-lightshow like), the entities just aren’t there in that I can sense no trace of them (it feels very impersonal, yet not ‘cold’ in the sense of the word) and the appearance and taste are virtually the same (one type may be slightly more chunky, but this is due to how fast it crystallised out). So all in all: yes, this is good spice. I assume it is >95% DMT. But it just isn’t what I prefer. The state of torpor my body wants to slip into in the residual-effect phase of the trip is just too much for me to handle. I hate the feeling of a very active mind (and it is active while on and after the trip) in an essentially paralysed and comatose body. I will not consume more of this in my ‘reverse order’ test that I am going to start in few days time. I’ve smoked 4 different kinds of this stuff, and I have enough for now. What I will do some time however, is smoke 60 mg of it. Perhaps there is some kind synergy going on that will blow me out of the water. I will combine these, save half a vial of it and use the rest in re-crystallization experiments, which is something I have never done yet, only inorganically with aluminium-salts. It should be great fun!
The pictures above are of the exact same dish. The spice is just spread out differently.
JimJam reduction (it’s a dirty job, but somebody’s got to do it)
An amount of 1.00 g of
combined JJS was dissolved in 50 ml of 36% acetic acid. Not everything dissolved; a lot of muck kept being afloat on the top and sticking to the glass. The solution remained cloudy as well. Added 2.0 g of Zn-powder. A pretty decent effervescent reaction set in, along with that same faecal smell as before. This time, the solution neither went colourless (it became a greenish-yellow) nor clear (it stayed rather cloudy). It was left to react for 5 hours (got held up in an appointment) during which time the vessels’ contents lost 0.75 g of mass. It was then decanted and filtered. An amount of 1.75 g of zinc was recovered. My now empty reaction vessel smelled of perfume <sighs>.
The acidic, polar solution was transferred to a 100 ml separating funnel and was extracted with 3 x 10 ml of naphtha (to get rid of unreacted materials, specifically my fabric softener oils). The naphtha extracts were discarded and the now clean, but not entirely clear solution transferred to the larger separating funnel, where it was neutralized with 30% NaOH solution and brought to pH8.
Note: This was the original recipe; 30% lye. On retrospect, this is unworkably strong. I overshot the pH8 mark by a long way and had to re-acidify with acetic acid. Using a dropper, I could get it to pH8 again, but it proves far to fiddly for comfort. Better switch to 10% lye or less when approaching neutrality! This fuckup
might also be the reason for what happened next:
This milky solution was extracted with 20 ml portions of naphtha. At the first portion, it became apparent that the dreaded “floating hydroxides” had returned: a white emulsion-layer at the surface consisting of naphtha, spice, water and Zn(OH)2 semi-solids. It will be dealt with as before. Persevere, and be patient: nothing is changed physically, only chemically. And this means that it’s reversible, not matter how big the fuckup. I apologize if the following paragraphs read more like a recipe than an account of observations, but this matter has been asked about so often in the forum, I thought this best. The volumes stated here are my volumes, yours will no doubt be different.
Cracking the emulsions
Basically, to separate any solvent from an emulsion that has formed, you use warmth, salt and mechanical means to split the mix into their constituents. Always try to get the bottom-‘clear’ in one beaker, the middle-‘muck’ in another, and the top-‘solvent’ in a third. Make sure the top and the bottom fractions are indeed clear. Everything not clear should go in the middle beaker, by definition. Adding heaps of salts to a polar/non-polar emulsion works wonders; it will make the polar part even more polar, forcing more non-polar solvent out of the emulsion. Don’t skimp on the salts, but never let the whole volume solidify. And never add salts to anything when it is in the separating funnel: you’ll just clog up your cock.
You need 4 beakers in addition to the separating funnel your problematic mix is in. Put 3 beakers in front of you, left – middle – right. I use these terms and positions to avoid confusion. Make the middle beaker a litre-sized one. Separate as much of the clear, watery solution at the bottom as possible and set aside in a separate fourth beaker for later. If there’s a small amount of white at the very bottom, put it in the centre beaker first. Put the floating white muck (about 40 ml) in the middle beaker. Any clear naphtha goes in the left beaker. You now have an empty separating funnel so put it aside for later.
Add several heaping teaspoons of anhydrous Na2CO3 to the middle beaker. Let it sink to the bottom, then stir and swirl vigorously. Warmth from the exothermic reaction, centrifugal force and the overload of salts separate out some of the naphtha, which is decanted into the small beaker on the left. Do not attempt to decant too much, or you’ll get too much emulsion in the left beaker with the naphtha. More soda is added to the middle, more swirling, more naphtha split off from the gel, decant into the left. Repeat this until you have about 75% ml of the naphtha thought to be in the mix (with a bit of emulsion) in the left, and a beaker in the middle with chunky soda-mud that won’t dissolve any further without adding more water. Add 50 ml of water to the middle mud and swirl for several minutes. Decant into the (up until now) empty right beaker. Add piping hot tap-water to centre beaker and dissolve rest of crystals. Add it all to the right beaker. Transfer this right beaker’s contents (clear water) to the separating funnel. Right beaker and middle beaker are now empty. Add 20 ml of naphtha to funnel and extract. Drain clear water portion-wise into right until a thick gel of naphtha and water remains. Swirl sep-funnel. This will dislodge some naphtha from the mix and put a few mm of clear liquid at the bottom of the funnel. Drain this clear liquid into the right beaker. If applicable, drain some of the emulsion in the centre beaker and do the heaping teaspoons and dissolving routine as earlier. Back to the separating funnel: swirl some more. Repeat. You are left with 20+ ml of naphtha over a few ml of thick emulsion/gel. Dump this in the left beaker.
You now have 40 ml of spice-containing naphtha and about 10 ml of semi-solid gel. Put gel together with right beakers’ contents PLUS the clear that was separated in the first step (it should milk up on you good) PLUS any other clear that you may or may not have in the big sep-funnel and re-extract with 20 ml of naphtha. Separation should proceed pretty normal now. Use the swirling technique to get a better separation, but only when there is just the gel left in the funnel; clear and muck should be in their respective beakers. Again, the mechanism at work here is centrifugal force together with friction on the glass. This is why it works best in a nice, rounded separating funnel shaped like a cone.
With all this sodium carbonate added, the pH of the solution should be 12 or higher by now. Extract using the above techniques as needed with 3 x 20 ml of naphtha. I should mention at this point that this is the first time EVER that I have seen yellow naphtha. Often it has been described here at the Nexus, but it has been a myth for me until now: PMS 108 FTW! I like the yellow spice better than the white, so far. No, I don’t have a dog.
After drying I ended up with 77 g of naphtha, equalling about 120 ml. A bit too much for holding just 1 gram of spice. I let it evaporate in a large flat dish overnight to 48 g, or 75 ml. That went faster than I wished for! Small crystals could be seen on the bottom of the dish, meaning I should end up with about 0.75 g of spice, because that is the concentration it should start to crash out on me. Then again, all crystals can start forming from any rough edge on the glass’ surface, so I ‘m probably too optimistic here. At any rate, I wanted it all into solution again, so I warmed the dish au-bain-marie, dissolving the crystals. I transferred it, rinsing with fresh naphtha, to the freeze-beaker. It was 57,5 g or 90 ml. Perfect.
Still, it’s interesting to note that the solubility of DMT in naphtha at room-temperature is around the 10 g per litre-mark (could be more though). At freezing, this is reduced to 250 mg per litre maximum, as per my own findings. My Coleman-naphtha deposits >97.5% of it’s dissolved DMT in my freezer. Nice!
The beaker was first put into the fridge at 5 degrees for 8 hours, then into the freezer for 24 hours. What came out of that was an amount of large, quite yellow crystals (PMS 114) that were very easy to scrape out of the beaker once I decanted the naphtha, leaving hardly any smears. I got 0.52 g of crystal freebase, or 52 %. Let’s crunch these numbers: On average I recovered 82% of
JJS as fumarates before. Of those fumarates, in
process C, I recovered 66% as freebase in the form most valued by me personally. 66% of 82% is 54%. I got 52% in this
JJS-to-freebase experiment, so I am inclined to say I got the same yield here. Which is nice. All this also means that whatever it is that produces this yellow colour:
a. It is organic,
b. It is not “converted” by Zn-reduction (hallelujah!),
c. It switches between salt/base form under the same circumstances as DMT does,
d. It is, like DMT, not decomposed by relatively strong acids or bases,
e. It makes up 5% or less of the total mass of the spice,
f. It is about equally soluble in naphtha as spice is.
The naphtha from the freezing was completely colourless whereas before it was a definite yellow PMS 108, meaning that all the yellow is now in the spice. Good or bad? Remains to be felt. I used this freeze-naphtha to dissolve any and all remains of spice in the beaker and on the tools I just used (a tablespoon, a teaspoon and an analytical spatula), and after evaporating it I was left with 35 mg of an amorphous mass that, alongside the strong spice-smell, very vaguely smelt of my dreaded softener (hello darkness my old friend…).
When I think back on it, I think there was a unique moment in time, the moment the spice just came out of the freezer and was air-drying, when I could have done something about the colour: It’s possible that for a minute or so, the ‘colour’ was liquid while the spice was not. I could swear I could see the colour drain from a few of the agglomerations of crystals into their neighbouring crystals by what looked to me like capillary action; the several ‘white’ clumps you see in the photograph. If I had let it drain on filter paper, they might have turned out more white, and I would have some of that mystery component concentrated in a piece of paper…. Next time, Gadget?
Bodymind: Holy shit! This went pretty deep. It had all the techno of white DMT, but with a more organic feel to it. What I especially liked, where the glimpses of completely different, realistic scenes that popped up for half a second at a time like small panels in a stained-glass window doing an “opening and closing the blinds”-effect. There were a lot of those, and I hope to one day penetrate that cell and really step into those scenes that so tentatively flash themselves to me. What I didn’t like however, were the body-shakes and the excessive yawning I got. I felt like a junkie in a cold-turkey abstention phase. The shakes went on and on in the end-phase of the trip, greatly disrupting the flow of it. And I wasn’t feeling cold, not consciously anyway. I yawned so much I felt my jaw was gonna crack. This was a very strong bodyload to carry, and I think I don’t like this spice because of it. I did however cry tears until my face was wet. And this I like. Also, because it was all so disrupting, I stood up and walked to the bathroom to get a glass of water. I looked absolutely fine in the mirror; I was even smiling while it didn’t feel like I was smiling. I also craved chocolate afterwards, and got me a bar of LoveChock (Dutch brand of organic cold-milled chocolate with nibs in it). These have a little message inside the package, like a Chinese fortune cookie. It read: “I overcome any fear with the power of my heart”. How true.. I ate the bar in 5 minutes.
Entities: None, unfortunately. The visuals too, were impersonal. But Very Beautiful.
Taste/appearance: Great taste, but the aftertaste was definitely ‘spicy’ in that it was like Capsaicin in mouth. That’s also why I went for that glass of water. Not entirely unpleasant, but very unexpected. The colour and texture of this spice was great! Very high density and a dream to handle.
Verdict: I am torn. On the one hand it is too much like my other Zn-reduced spice. But on the other hand it seems there are great things waiting to be discovered. I am just not sure I can handle a double-dose of these bodily effects.. I hope they stay at the same level when I double up a next time…
