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washing freebase DMT? Options
 
artificer
#1 Posted : 8/28/2021 8:30:36 PM

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Another A/B extract done, using Vovin's Tek as in the past, but, regrettably, the sodium carbonate wash step was skipped this time (in the previous batches it was done but got cloudier instead of clearer like the Tek described).

It is suspected that NaOH is in final product - details and pics below - but straight to the question: What are top options to obtain clean product from FB DMT that likely includes NaOH?

I've been reading through guides and TEKs and Wiki and queried for "wash" + "NaOH", etc and perhaps I looked right over the info I needed, but I didn't find something clearly stating that a specific process or wash would retain majority of DMT and leave behind the NaOH.

I've tried freeze precip a number of times and maybe I just need to find right process but I get frustrated with partial product precipitated and partially still dissolved and the H20 condensation getting into solution, and I can't determine from what I've read whether or not the freeze precip would leave behind NaOH anyway.

ReX is fine but I don't have experience yet with that and again I can't determine if that would get rid of NaOH.

I'm assuming that dissolving in hot naptha and throwing that in seperatory funnel with sodium carbonate H2O followed by pure H2O washes would do the trick, but I'm worried about losing more DMT than necessary in the process.

If I followed process to convert to DMT fumerate with dry acetone and fumaric acid, would this remove the NaOH? If not, would the steps to convert fumerate back to FB (with calcium hydroxide or calcium carbonate) do the trick?

Details: 1,300mg of product was obtained from 100g MHRB using Vovin's A/B tek, this is in the larger/left jar in pic. Smaller jar on right is what's left from previous batch. appearance is slightly different, but the main reasons I suspect NaOH in large jar is that the small jar has much sweeter smell and stronger scent of mothballs, and I put smallest amount from large jar to my lips/tongue and it presented as tingly/chemical taste, like I imagine caustic soda would.

Thanks in advance for any advice here...
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downwardsfromzero
#2 Posted : 8/28/2021 8:53:34 PM

Boundary condition

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Converting to the fumarate would also convert any NaOH to sodium fumarate.

Quote:

Details: 1,300mg of product was obtained from 100g MHRB using Vovin's A/B tek, this is in the larger/left jar in pic. Smaller jar on right is what's left from previous batch. appearance is slightly different, but the main reasons I suspect NaOH in large jar is that the small jar has much sweeter smell and stronger scent of mothballs, and I put smallest amount from large jar to my lips/tongue and it presented as tingly/chemical taste, like I imagine caustic soda would.
NaOH produces a soapy feel and taste, through literally turning you into soap just before the agony kicks in in the case of larger amounts.

DMT itself is a strongly basic amine so it will have some caustic properties in higher concentrations (such as the crystal). As far as odour goes, lack of any smell is more a sign of purity - the mothball smell comes from contaminants such as indole. Very pure DMT will smell faintly sweet with the barest floral hint from inevitable decomposition.

Why would you think that NaOH would make its way through the non-polar phase? Did you make an emulsion during the extraction?




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
artificer
#3 Posted : 8/28/2021 9:26:45 PM

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Quote:
Why would you think that NaOH would make its way through the non-polar phase? Did you make an emulsion during the extraction?


Rationally through what I understand of the process, I don't have logic to make me think that NaOH would've made its' way through non-polar phase. It's more of a fear... I realize that Vovin's Tek is older but it does include that wash step with sodium carbonate (step 9: solvent wash)

During the naptha pulls I think it would be called emulsion as I was using 2L separatory funnel with 1L of liquid sloshing perhaps more violently than it should, however, I transferred collection of Naptha from pulls to smaller separatory funnel to remove anything not clear and again to another jar where I believe I got all visible drops of basic solution to be left behind.

Based on your reply, it seems I've got better product not worse than previous batch... fingers crossed. I still have 200mL of xylene to try FASA tek on for first time for the jungle spice...

Quote:
Very pure DMT will smell faintly sweet with the barest florall hint from inevitable decomposition.

^^This is how it smells^^

"inevitable decomposition" brings me to another question I haven't found clear answer to: how quickly will the FB break down? I keep it in infinity jars, and could put in vacuum if that would help significantly. Will a gram of FB be noticeably weaker in 6 months? I'll do fumerate conversion and/or extract anyway for MOA other than smoking, but I'll always want some FB for smoalking.

appreciate the help dfz
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downwardsfromzero
#4 Posted : 8/29/2021 2:06:22 AM

Boundary condition

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One alternative approach, for future reference, is to wash the naphtha pulls with strong brine before the freeze precip. That would remove traces of NaOH solution from the naphtha along with reducing the moisture content and should contribute to giving a cleaner-looking, more stable producct.

The brown discoloration often seen is thought to be due to oligomerisation which is catalysed by moisture and traces of base.

Your DMT will happily keep for 6 months. Discoloration will be limited to the surface - both the colour and the odour are very potent so it's only a negligible amount of your product that will have been affected. For longer term storage an inert atmosphere would be preferable to vacuum as DMT is fairly volatile. Optimum storage conditions were outlined recently in this thread.




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
artificer
#5 Posted : 8/29/2021 4:08:27 AM

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Quote:
One alternative approach, for future reference, is to wash the naphtha pulls with strong brine before the freeze precip

When you say "strong brine", do you mean it in the common sense, as in saltwater?

Quote:
The brown discoloration often seen is thought to be due to oligomerisation which is catalysed by moisture and traces of base

this is interesting, for two reasons

1 - I had to look up oligomerisation. I wonder, in this case, if it's homo- or hetero- oligomer? I'm no chemist (yet) but it intrigues me.

2 - The first go-around with this batch I evaporated 500mL+ of naptha inside, with hepa-filter/fan setup pulling air from inside and blowing at the evap dish and out the window, while unavoidably pulling fresh air from outside from another window. humidity went through the roof, the dried product was relatively red/brown/yellow gooey. I dissolved this with <100mL fresh, warm naptha and evaporated this small amount with windows closed and 48% relative humidity, the final product is now more white and less gooey.

there might be more I meant to say here.. but the mushrooms are kicking in...


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downwardsfromzero
#6 Posted : 8/29/2021 4:08:40 PM

Boundary condition

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Quote:
When you say "strong brine", do you mean it in the common sense, as in saltwater?
Indeed.

The other thing to bear in mind is that DMT has at least two polymorphs.

Your result with high humidity evaporation vs. that of the lower humidity has the additional difference that a larger volume of solvent will evaporate more slowly, resulting in greater exposure to atmospheric oxygen both in terms of time and also because the DMT will be spread out over a bigger area.

Hope you had a good trip last night Smile




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Hailstorm
#7 Posted : 9/13/2021 12:03:44 AM

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artificer wrote:
What are top options to obtain clean product from FB DMT that likely includes NaOH?

I'd recommend a wash with freezer-cold ammonia, also known as ammonium hydroxide - as concentrated as possible (28% is good).

If it is concentrated and fresh (ammonia easily escapes from containers, so check the pH) it is sufficiently alkaline, so it will not make DMT water-soluble. It contains enough water for NaOH to dissolve in.

Best of all, ammonia is a gas so it evaporates completely, leaving no residue unlike sodium carbonate.
 
 
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