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Noman extraction failed again, I'm going to cry :( Options
 
5A8R3
#1 Posted : 3/9/2019 7:53:40 AM
Followed Noman's tek almost to a T.

Using de-ionised de-mineralised water.
Tested my base solution with litmus, was above 12 pH.
Soaked powedered bark for 24 hours with agitation.
Only did 2 pulls due to freezer space, but I assumed first pull takes most out anyway so it shouldn't prevent precipitation?

Freeze precip for 12 hours. Check jars, naptha is cloudy with some wispy clouds if I agitated the liquid. Whyyyyyy? Could be because the naptha has been used once before...

So I dump a load of dishwashed salt (salt without anti-caking agent??) mixed with a whisk and do another 2 pulls with fresh naptha.
Freeze precip again for 12 hours, same wispy cloud result.

I am going to cry Sad
Is it possible the first 2 pulls took some crystal but not enough to induce precipitation, which then meant the following 2 pulls with fresh naptha also didnt have enough crystal to successfully precip?

I don't know what the hell I am doing wrong, should I use more lye next time to make sure the bark is breaking down?
Is there a problem with adding excessive lye?

*Sobs*

Exact measurements:
5 Ltr De-Ionised water
380g Lye
350g Powdered Bark
350ml + 350 ml + 100ml Naptha

Second attempt was added 500g salt which seemed to all dissolve...

Any ideas will be appreciated because I'm about ready to ditch this tek for something more reliable.
 
RoundAbout
#2 Posted : 3/9/2019 6:17:25 PM
5A8R3 wrote:
I am going to cry Sad Is it possible the first 2 pulls took some crystal but not enough to induce precipitation, which then meant the following 2 pulls with fresh naptha also didnt have enough crystal to successfully precip?


Fresh solvent will probably pull more DMT, but many people reuse naphtha that has been used for freeze crystallization (without distilling first). You're also using large volumes of naphtha to pull (more smaller pulls are more effective, though perhaps this is fine with your ratios).

My first thought is that perhaps the DMT concentration in the naphtha is simply too low, and my suggestion is to combine all the naphtha and evaporate at room temperature until it is just slightly cloudy (i.e. increase the concentration and nucleate), and then put it in the freezer (i.e. decrease the solubility and crystallize).

Edit: As downwardsfromzero said, a mini A/B is far better than evaporating.
 
downwardsfromzero
ModeratorChemical expert
#3 Posted : 3/9/2019 9:14:24 PM
Yeah that is loads of naphtha. No need to evaporate. recover with a mini A/B of sorts - backsalt it into vinegar, add base and pull again with way less naphtha. Lots of small pulls are better than one big one. They can be combined afterwards to save space in the freezer.

If your freezer is cold enough (-18°C or less) that should work; otherwise it's bunk bark.

Were you using MHRB?




“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
 
5A8R3
#4 Posted : 3/10/2019 1:09:00 AM
Yes, it is MHRB.

Noman's tek calls for each pull to have 1 ml naptha per gram of bark, so the ratios are following the tek. So I should use maybe half the naptha but with many more pulls in subsequent extracts?

I'm not clear on what you suggest with the A/B recovery... I can migrate the the dmt from the naptha back into an acid, then base it and pull again?

Currenty I have 800ml of naptha that I was ready to ditch even though Im sure there is dmt in there, evap was what I was thinking but I'm interested if you could elaborate on a better way to recover what might be there...

Really appreciate the help.
 
downwardsfromzero
ModeratorChemical expert
#5 Posted : 3/10/2019 1:12:39 AM
Quote:
I can migrate the the dmt from the naptha back into an acid, then base it and pull again?

Yes, exactly that.




“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
 
5A8R3
#6 Posted : 3/10/2019 1:29:53 AM
Fantastic!
Ideal volume of acid and pH range?
 
5A8R3
#7 Posted : 3/10/2019 12:35:37 PM
So in theory there should be around 3g of dmt dissolved in SWIMs 800ml naptha.

I have no idea so I would just be guessing on how to do this.

Cracked out my new digital pH meter, strangely reading distilled malt vinegar as ph 2 whereas litmus paper is showing between 4-5. Common knowledge says most vinegars are 2.5 to 3.5 so I will have to assume my pH meter is not calibrated correctly and also that the vinegar I have is around 3 pH.

So looking at Lextek so try and discern quantities, it looks like 50ml of acid per 1g of dmt is appropriate. If this is true I should use 150ml, with maybe 50ml extra to give more room for dmt to dissolve into the acid?
No idea also if I should place naptha and all of acid into container and shake or will it emulsify so should I instead do multiple acid pulls?

Then maybe 5 pulls of 50ml naptha after basing to +10pH.

Sound good?

I'm probably going to look into FASA after this debacle
 
null24
Welcoming committeeModerator
#8 Posted : 3/10/2019 3:39:01 PM
5A8R3 wrote:
So in theory there should be around 3g of dmt dissolved in SWIMs 800ml naptha.

I have no idea so I would just be guessing on how to do this.

Cracked out my new digital pH meter, strangely reading distilled malt vinegar as ph 2 whereas litmus paper is showing between 4-5. Common knowledge says most vinegars are 2.5 to 3.5 so I will have to assume my pH meter is not calibrated correctly and also that the vinegar I have is around 3 pH.

So looking at Lextek so try and discern quantities, it looks like 50ml of acid per 1g of dmt is appropriate. If this is true I should use 150ml, with maybe 50ml extra to give more room for dmt to dissolve into the acid?
No idea also if I should place naptha and all of acid into container and shake or will it emulsify so should I instead do multiple acid pulls?

Then maybe 5 pulls of 50ml naptha after basing to +10pH.

Sound good?

I'm probably going to look into FASA after this debacle

I think you may be over thinking things. If you want experience extracting, try a tried and true tek for beginners like cybs. Once you get a feel for what you're doing, your volumes won't be such a big matter of concern, you'll just know what works.

The only thing i know about lextek is that it was written a long time ago.

Good luck with a FASA if you're having trouble with AtB...
Sine experientia nihil sufficienter sciri potest -Roger Bacon
*γνῶθι σεαυτόν*
 
5A8R3
#9 Posted : 3/10/2019 4:32:49 PM
null24 wrote:

I think you may be over thinking things. If you want experience extracting, try a tried and true tek for beginners like cybs. Once you get a feel for what you're doing, your volumes won't be such a big matter of concern, you'll just know what works.

The only thing i know about lextek is that it was written a long time ago.

Good luck with a FASA if you're having trouble with AtB...


I'm trying to avoid use of the kitchen whcih is why Noman's tek was appealing. I have been successfull a few times previously but the last few times was not, since I scaled up the ratios. I just wanted to clarify the A/B procedure as I haven't done it before.

Anyway, the advice given so far has been very usefull so many thanks.
I'm going to wing the A/B and see what happens.

IF
Quote:
At 20 °C one liter of water can dissolve about 357 grams of salt, a concentration of 26.3%. At boiling (100 °C) the amount that can be dissolved in one liter of water increases to about 391 grams, a concentration of 28.1%

AND
Quote:
It should take only about 20–30mL of solvent per gram of powder

THEN I figure I should use about 150ml naptha to recover this dmt from the acid

No idea how much acid, I'll just use 300ml and see if it works.
 
Shnuffles
#10 Posted : 3/10/2019 9:27:55 PM
So this is my method for extracting DMT from MHRB, based on what I have found to be the most useful parts of several other STB teks, as well as my own research and experience. I am a perfectionist and love science projects, so I tend to be very thorough, and so many of these steps are not entirely necessary but I find them to be beneficial to my final product. I'm sure there are things i have missed, as this is an early draft of what i hope to eventually be my own tek, so always do your own additional research as well in case i, or anyone else, for that matter, missed anything.

Safety-wise, always work in a well ventilated area when working with volatile solvents, such as naptha, and always wear long sleeves, long pants, and appropriate protective gloves, footwear, and goggles when handling these things in case of any accidents. Also in case of any accidents, always keep a large bottle of vinegar nearby in case of any lye spills, and make sure it is easily opened and quickly accessible. Again, i may be missing a few things, so always do your own additional research before attempting to work with these potentially hazardous substances.

1. Prep

a) Preparing your bark.

-Freeze your bark as cold as your freezer will allow. After 4-12 hours of initial freeze time, you can either break it up by hand to save your blender some wear and tear, or you can just go straight to the blender.

-Take small amounts out of the freezer at a time and break up your bark by hand as much as possible. Since it is frozen, this should not be difficult, especially with a small pair of garden clippers or a pair of strong scissors. As you finish breaking up bark, place it back into the freezer while you systematically break up the rest. Once this is all broken up, personally, i like to take it all back out of the freezer, let it thaw, and refreeze it, repeating this several times. Again, this may be overkill, but the more you do this, the more the cellular structure of the bark breaks open, creating less work for your base to break it down once it is fully powdered.

-Blend your bark. While it is frozen, place small amounts of bark into your blender and begin to pulverize them. To save your blender some work and wear and tear, on occasion, stop the blending process long enough for the dust inside to settle(~5-15 minutes should be sufficient) and carefully open it, carefully removing the powder into whatever collection vessel you choose to use. It is important that you let the dust settle before opening it. In the past, i have opened it early out of impatience throughout the process to remove the powder, and ended up losing ~5g of bark out of the 50 i started with. Continue with this blending process, adding more frozen bark as necessary, until it is all powdered. Often you may find a little tumbleweed of unblendable bark fiber in your blender; you can either refreeze it and powder it further, or just add it to the lye water when it is time to do so.

b) Mix your lye solution.

-Generally, most teks recommend using 500-750 mL of water and 1 g of lye for every gram of mhrb, however, i find that any more than 600 mL of water to be too much liquid to work with in the size of mason jars i use, and since the ratio is supposed to create a specific pH level, i say just skip the ratios and buy a pack of pH paper from a garden store, adding enough lye to the water to reach at least a pH of 13.

-IMPORTANT: ALWAYS MAKE SURE TO ADD LYE TO WATER, NEVER ADD WATER TO LYE!!!!! This can cause a violent reaction if done incorrectly!!!

-Also, be aware that the water heats up and can easily boil if you add the lye too quickly, so make sure you add it slowly to a vessel that is appropriate for such things, like a pyrex flask or a very clean empty patron bottle, for example.

2. Add the powdered bark to your lye solution.

-Place your lye solution into your extraction vessel

-Add your bark to the lye solution. Personally, i usually dont do more than 50 g of bark per vessel. This seems to provide a higher yield over more bulky extractions targeting 100+ grams of bark per extraction vessel

-Mix the two using a glass stir rod or your glass turkey baster

-Cover the mixture with doubled up plastic Ziploc-brand samdwich bags(much stronger plastic than other bags) and seal it with a rubber band or two. This way, if there is any gas expansion or pressure changes of any sort, it wont damage the vessel.

-Leave to dissolve for at least an hour or two, but preferably overnight, carefully swirling the jar on occasion.

3. Pulling with naptha

-For your first few pulls, if you are looking for as pure of a product as possible, do not use heat until your last few steps just to squeeze the last bits of spice out of the mimosa soup.

-For the first pull, take a small amount of naptha, preferably approximately 60-100 mL naptha per 500-600 mL of water, and add it to your mimosa/lye mixture. Replace the ziploc baggie(s) without the rubber bands, and replace the actual mason jar lid and screw top over the top of the baggie(s) in such a way that the plastic protects the lid(and therefore also the rubber seal on the lid) from exposure to any of the chemicals being used

-Note: I realize that ziploc baggies are made out of a plastic that is technically soluble in naptha, however, in the minimal amount of contact with the naptha and frequent changing of the baggies, i have personally never noticed any degradations in the baggies or impurities in the final product, although it is true that the final product could still have sone and i just dont notice it

-Shake, shake, shake that jar vigorously. Make sure that it is as well mixed as possible and then some. Emulsions are not as much of an issue with mhrb. However, if you do get emulsions, place the vessel in a warm(NOT hot) water bath, and it should separate fairly quickly.

-When you are done shaking it, make SURE to remove the lid and screw top, leaving only the plastic baggies behind, and, if they are damaged, replace them, and place the rubber bands back over the baggies to seal the lid, in such a way that if there is a pressure buildup or drop, it wil only flex the plastic and possibly be realeased from the sides through the rubber band seal.

-Leave it to separate for approximately 15 minutes, or up to an hour, and shake again. After about 4-6 shaking cycles, leave it to separate for at least an hour, maybe 3 or 4, and then do your pull.

-Before pulling, be sure to have your glass turkey baster nearby, as well as a thin, round-bottom vessel, such as a shot glass(DO NOT use this shot glass for ANY OTHER PURPOSE afterward, no matter how well you clean it, it is still possibly pretty toxic)

-To perform a pull, take your turkey baster, press on the bulb on only one side with a finger or thumb, then place the nozzle into the approximate center of the naptha later, preferably at an angle so as to draw up as little of the mimosa layer below as possible. SLOWLY release the pressure on the bulb with your finger, and if any of the lye mixture accidentally comes up with it, just let the tip of the baster sit in the middle of the naptha layer, still at an angle, and most of it should slowly leave the tip of the baster. If any does remain, which will be more and more likely as you pull more and more of the naptha layer out, place it into the shot glass or thin vessel. Once you have gone through a majority of the naptha and can no longer pull any more out, you likely will have had enough lye pull up with the naptha to fill the shot glass a fair amount, and it should be easier to further separate the remaining liquids in this vessel. Now your naptha is ready for freeze precipitation, which you will want to do only one or two pulls at a time to monitor progress and decide how many pulls to do. The freeze precipitation stage will be discussed further in Step 4

-Repeat this pulling process until your yield(after freeze precipitation) is no longer "worth it", then begin placing the extraction vessel in a warm(NOT hot) water bath after shaking, as previously discussed. This will pull the final remaining bits of spice out of the bark mixture, along with accompanying plant fats, as previously mentioned. Continue to do this until you no longer find the yeilded results to be worth the effort. As a general rule of thumb, you should be getting between 1%(good/normal) and 2%(great) yield in total between all if the pulls.

4. Freeze Precipitation

-Place pulled naptha into a glass dish with a flat bottom, and cover it up VERY WELL. It is best if you use a dish that comes with its own lid so that you know it wont leak fumes. If you do not cover it properly, your freezer and everything in it will smell heavily of naptha and have a thin coat of naptha covering it, and the only way to fix or get rid of this is to defrost your freezer, and honestly i would just throw all that food away. You dont want to accidentally consume naptha. So make sure you seal it properly.

-Once the dish with the naptha in it is sealed properly, place it in the freezer, trying to put it in the coldest spot possible.

-Ideally, your freezer should be set cold enough to freeze ice cream HARD(or so i have been told), and if it doesnt, it will still work, but you may want to evaporate all of your naptha used in the process after you are done to retrieve any lost spice.

-Leave your precipitation dish in the freezer, undisturbed, for at least 24 hours(less if you're freezer is high performance). Try your best not to open your freezer door during this time to guarentee the coldest possible temperatures. This step is why you don't want to use a lot of naptha for your pulls in the first place, because the less you use, the more of the pulled dmt precipitates, and the less you have to evaporate later.

-Remove the precipitation vessel from the freezer. When you remove it, many people are tempted to immediately pop off the lid and pour or siphon off the liquid as quickly as possible. DO NOT DO THIS. Immediately after removing it from the freezer, both the naptha and container are below the freezing temperature of water, and so any humidity in the air will condense on your naptha and on your precipitation dish, forming a sticky goo and little ice crystals forming on the surface of the naptha that looks like floating dmt crystals but it is NOT. Instead, WAIT FOR THE DISH TO REACH ROOM TEMPERATURE. You can tell this when you no longer see condensation on the outside of the container. It is common for people to think that if the naptha raises back to room temperature, it will redissolve the dmt, however this is simply not true. The naptha needs additional heat to redissolve the dmt, so at room temperature, it should be perfectly fine.

-Once the dish is at room temperature, carefully remove the lid, trying not to jostle the naptha too much, which could dislodge some dmt crystals from the bottom, making it slightly more difficult to siphon or pour off the naptha, trying not to lose those loose crystals.

-Use your turkey baster to carefully remove the naptha from the dish, and carefully pour off whatever is left over.

-Leave crystals to dry before scraping them up. When there is no longer a smell, you can start scraping, then spread them back out to further dry. Do not use a fan to do this. Ive read mixed opinions on this, but to be safe, i try not to use a fan when i do this because it supposedly could convert to dmt-oxide more quickly, or at the very least, the fan could dislodge and blow crystals around.



Once this process is finished, your spice is ready to do whatever you want to with it, and you can repeat the process as much as you like! You should get anywhere from 500 mg up to a gram of dmt from this process, generally speaking, so if you didnt get that much, either your bark has degraded or you still have more left to extract. Repeat this pulling and precipitating process until you have gotten as much spice as possible out of it. You can reuse your naptha several times, so at the end, you can evaporate the rest off to get back whatever never precipitated.

As previously mentioned, this is an early draft of what i hope to eventually be a tek, so if anyone has any feedback or notes, please let me know. I am certainly not an expert, nor do i pretend to be, so any and all input is very welcomed and appreciated.
I come from a place beyond the clouds. Only Shponglese is spoken there, and that is my native language. I am only just learning english, so if i say anything strange, it is probably a miscommunication on my part and i apologize. I sdsrrrbablenta to all of you and i ghope tjat you can forgive any miscommunications.

May the Elves ever be in your favor,

~~~Shnuffles
 
5A8R3
#11 Posted : 3/10/2019 10:13:16 PM
Well, what an interesting process!
I miss-spoke before as it was a total of 1.6 L of naptha to deal with.

Anyway, added 300 ml of vinegar to naptha bottle, which became cloudy immediately. Pleased to see no emulsion formed I shook vigorously and noticed the vinegar turning pale yellow. Interested to see what the cloudines of the naptha was about I added the remaining 100ml of vinegar I had and shook like mad. Naptha did become less cloudy but not totally clear so not sure what is going on there.

Was was quite perculiar was a layer that formed between the acid and the naptha that looked like an emulsion but when I eventually separated this layer it had a snotty consistency and smelled faintly of dmt. So I am guessing this is some kind of fat that didnt dissolve in either layer. If so that is a great added bonus as it has been removed.

Totally awesome watching the solution turn cloudy in an instant as I was adding the lye. Whatever was there really didn't want to be in that base solution as it settled it formed into particles.

Also really interesting watching the solution become more and more clear after each pull.

So I have high hopes now as I put 400ml of naptha into the freezer Smile
Thanks again for all advice.

As for Snuffles' post:
I agree with most of your techniques and especially find the idea of leaving the precipitated solution to reach room temperature before proceeding. I've always filtered it immediately and had both results - completely wihte fluffy crystals as well as some oily results; I always thought that was jsut the result of plant fat entering the naptha on some occasions, especially if the naptha had been left in contact for a long time.

What I think could be improved about the wiki page for Noman's Tek is a clearer understanding of why the ratios used are as such. As you mentioned Shunffles
Shnuffles wrote:

Generally, most teks recommend using 500-750 mL of water and 1 g of lye for every gram of mhrb, however, i find that any more than 600 mL of water to be too much liquid to work with in the size of mason jars i use, and since the ratio is supposed to create a specific pH level, i say just skip the ratios and buy a pack of pH paper from a garden store, adding enough lye to the water to reach at least a pH of 13.


Me following the ratios when scaling up was the source of the problem in the resulting use of too much naptha.
So now I know as long as I hit that pH I can put a greater range of plant volume in there. So it begs the question as to why not pack double the MHRB into the same amount of solution. If I'm using 5 litres of water, maybe I could put 500-600g of bark in there istead of the recommended 330g.

Something that you didnt mention that I have noticed Shnuffles - you say to leave your dish to completely dry before removing the crystals. In contrast I have noticed that if I scrape the losser crystals off with a silicon spatula and place them to dry, this separates the purer crystals from the crystals that are stuck more heavily to the glass due to combination with the plant fat. So you can obtain two grades of crystal from the same precipitation. I suppsoe this might only work while it is still freezer cold though.
 
AcaciaConfusedYah
Chemical expertSenior Member
#12 Posted : 3/11/2019 4:27:52 AM
Seems to have already been addressed - but scaling was likely a big issue.

In short - maximum surface area exposure and contact time will be the factor in terms of efficiency.

I usually only perform ~50 gram extractions and try to "keep the aqueous small and the organic large." By small - i mean small volume of water and small quantities of sodium hydroxide (usually no more than 10 grams). I prefer to do less, and get more- so I do a single "large" pull (often 1/3rd the total volume [700 mL aqueous to ~250-300 mL organic]).

Freeze precipitation, and call it a day. Yielding around 1.5%; I've written it up, so it is out there if yah wanna see.

Good luck. Change your scaling next time. Less is more.
Sometimes it's good for a change. Other times it isn't.
 
Shnuffles
#13 Posted : 3/11/2019 6:51:49 AM
5A8R3 wrote:
So it begs the question as to why not pack double the MHRB into the same amount of solution. If I'm using 5 litres of water, maybe I could put 500-600g of bark in there istead of the recommended 330g.


I have wondered this myself, but i sort of feel like that would be too much bark in the same water, and it would get muddy and mucky, possibly thicker than what is usable for our purposes. For example i would think that this would allow for more frequent emulsions due to naotha getting trapped under all that bark.

5A8R3 wrote:
Something that you didnt mention that I have noticed Shnuffles - you say to leave your dish to completely dry before removing the crystals. In contrast I have noticed that if I scrape the losser crystals off with a silicon spatula and place them to dry, this separates the purer crystals from the crystals that are stuck more heavily to the glass due to combination with the plant fat. So you can obtain two grades of crystal from the same precipitation. I suppsoe this might only work while it is still freezer cold though.


I see what you are saying 5A8R3, but again, opening it so quickly after taking it out of the freezer invites moisture and condensation, so you will likely end up with a gooier product, and i dont see why what you describe would be exclusove to being only possible at freezer temps.

All in all, i agree with Acy, scaling seems to have been a major factor here. I mostly just gave my methodology for you to compare and contrast with yours and possibly troubleshoot that way. I find that most of the teks have the right information and each has something unique to bring to the table, so i just frankensteined what i found most useful and threw in some tips that i wish i had been told when i first started. By no means do i think my method is perfect or better than any others, but it has been what has worked for me. I do tend to overcomplicate things but in this case i believe i did fairly well
I come from a place beyond the clouds. Only Shponglese is spoken there, and that is my native language. I am only just learning english, so if i say anything strange, it is probably a miscommunication on my part and i apologize. I sdsrrrbablenta to all of you and i ghope tjat you can forgive any miscommunications.

May the Elves ever be in your favor,

~~~Shnuffles
 
 
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