Gooey ooey ooey, need precip help!

[WaffleStompN214]

After doing Norman’s trek using pre-powdered, its gooey blobs. I’ve tried using vacuum to try and fix it but that didn’t work. It’s not really yellow, and I didn’t get any soup in it(see pic) Any advice will be greatly appreciated
250g powdered mim
300g lye
1900ml distilled water
Then:
125ml naptha

 

[WaffleStompN214]

Another pic

 

[quantumtantra]

You should increase the chance of a good advice here by increasing the amount of details about your extractions paths, otherwise people will need to ask you questions before which is counterproductive.

 

[dreamer042]

A straight to base extraction like that will generally pull some plant fats/oils/resins along with the alkaloids. Did you complete the recrystallization step yet?

I generally add a backsalt/defat step prior to freeze precipitation to clean things up and I always complete at least one recrystallization.

 

[WaffleStompN214]

A straight to base extraction like that will generally pull some plant fats/oils/resins along with the alkaloids. Did you complete the recrystallization step yet?

I generally add a backsalt/defat step prior to freeze precipitation to clean things up and I always complete at least one recrystallization.

I have not. I wasn’t sure if I should do that while it was gooey. I actually just got a notification saying carbonate and hept have been delivered. Are the steps listed in Nomans the ones I should follow or is there a better source? Thanks a bunch for your help.

 

[WaffleStompN214]

A straight to base extraction like that will generally pull some plant fats/oils/resins along with the alkaloids. Did you complete the recrystallization step yet?

I generally add a backsalt/defat step prior to freeze precipitation to clean things up and I always complete at least one recrystallization.

What exactly does the backsalt/defat step prior to freeze consist of? Can I do it with my gooey results of freeze?

 

[WaffleStompN214]

You should increase the chance of a good advice here by increasing the amount of details about your extractions paths, otherwise people will need to ask you questions before which is counterproductive.

You should increase the chance of a good advice here by increasing the amount of details about your extractions paths, otherwise people will need to ask you questions before which is counterproductive.

Thanks. I added details of my experiment.

 

[drpotato]

What exactly does the backsalt/defat step prior to freeze consist of? Can I do it with my gooey results of freeze?

defat amounts to exploiting the fact that fats wont react with acid but dmt will. so you pretty much just do a pull or 2 on, normally your acidified soup.
NPS wont pull say, dmt acetate out of water, but the fats, it will.

 

[dreamer042]

For recrystallization, follow as outlined in Noman's

backsalt equates to: dissolve the material in vinegar water (50/50), pull with fresh naphtha (the alkaloids will stay in the acidic water layer and any impurities will pull into the solvent), discard the solvent. Base the acidic water again then proceed as before, 3 pulls, evap, precip.

 

[WaffleStompN214]

For recrystallization, follow as outlined in Noman's

backsalt equates to: dissolve the material in vinegar water (50/50), pull with fresh naphtha (the alkaloids will stay in the acidic water layer and any impurities will pull into the solvent), discard the solvent. Base the acidic water again then proceed as before, 3 pulls, evap, precip.

So this is done after the initial soaking in lye solution? 50/50 vinegar/water but how much of the solution? Would it be close to the same amount of water I used initially with the lye? In my case 1900ml?

 

[drpotato]

So this is done after the initial soaking in lye solution? 50/50 vinegar/water but how much of the solution? Would it be close to the same amount of water I used initially with the lye? In my case 1900ml?

no. because then you would need to neutralize the lye with vinegar, and then afterwards youd need to re-basify again. Granted, you *could* but, the molar mass of sodium hydroxide is 40g, while acetic acid is 60g, meaning it takes 3 parts by weight of pure acetic acid, to neutralize 2 parts sodium hydroxide. In 5% vinegar, and assuming acetic acid is exactly as dense as water, this works out for 5% of the stronger sort of cleaning vinegar, to require roughly 20x1.5 =30ml of cleaning vinegar to neutralize each gram of sodium hydroxide.
What you can do now though is run a mini AB on what you have. Im not sure how much vinegar to use but it wont be much really. dmt has a molar mass of 188g/Mol so, for every suspected gram of DMT there, you add 188/60 then times 20 for 5%, lets just call it 60ml vinegar. excess wont hurt so calculate it based on your expected best case scenario then add like 20-30% more or something. Otherwise, you should be able to tell using ph strips or a ph meter, the ph wont drop all the way down until the DMT is reacted, although it may take a little bit of time to actually react and do that. follow a tek for this not just what ive said, theres more to it.

I dont know who norman is or what their tek entails, they dont appear in the search engine, but, usually we start by acidifying the bark if we want to do a defat in the process. In a dry tek, which i assume is what this one is, we rely on a fairly pure source, and fairly good crystalization so that the crystals will form out of the fatty naptha, which you can then proceed to rinse away with additional cold naptha, to get acceptably pure spice, although the fats may themselves be solvating some DMT so while its an easy low effort method, the yield does suffer and the quality isnt as great as if the fat were omitted right from the outset.

Most teks balance yield, quality and complexity and sacrifice one for the other(s), MHRB generally contains nothing but DMT and trivial contaminants that are in low quantity and are easily removed.

On that note, take a ml of naptha and evaporate it on some glass and see if it leaves behind oil or not. you are supposed to check this anyway with your naptha source. its uncommon but it does happen.

 

[WaffleStompN214]

no. because then you would need to neutralize the lye with vinegar, and then afterwards youd need to re-basify again. Granted, you *could* but, the molar mass of sodium hydroxide is 40g, while acetic acid is 60g, meaning it takes 3 parts by weight of pure acetic acid, to neutralize 2 parts sodium hydroxide. In 5% vinegar, and assuming acetic acid is exactly as dense as water, this works out for 5% of the stronger sort of cleaning vinegar, to require roughly 20x1.5 =30ml of cleaning vinegar to neutralize each gram of sodium hydroxide.
What you can do now though is run a mini AB on what you have. Im not sure how much vinegar to use but it wont be much really. dmt has a molar mass of 188g/Mol so, for every suspected gram of DMT there, you add 188/60 then times 20 for 5%, lets just call it 60ml vinegar. excess wont hurt so calculate it based on your expected best case scenario then add like 20-30% more or something. Otherwise, you should be able to tell using ph strips or a ph meter, the ph wont drop all the way down until the DMT is reacted, although it may take a little bit of time to actually react and do that. follow a tek for this not just what ive said, theres more to it.

I dont know who norman is or what their tek entails, they dont appear in the search engine, but, usually we start by acidifying the bark if we want to do a defat in the process. In a dry tek, which i assume is what this one is, we rely on a fairly pure source, and fairly good crystalization so that the crystals will form out of the fatty naptha, which you can then proceed to rinse away with additional cold naptha, to get acceptably pure spice, although the fats may themselves be solvating some DMT so while its an easy low effort method, the yield does suffer and the quality isnt as great as if the fat were omitted right from the outset.

Most teks balance yield, quality and complexity and sacrifice one for the other(s), MHRB generally contains nothing but DMT and trivial contaminants that are in low quantity and are easily removed.

On that note, take a ml of naptha and evaporate it on some glass and see if it leaves behind oil or not. you are supposed to check this anyway with your naptha source. its uncommon but it does happen.

Thanks. A lot of this is like Chinese to me but I’ll try to translate your steps. I’ve only got a couple extractions under my belt and I’m not afraid to admit that I was just following directions. I want to learn the science behind it but for now I’m just doing s I’m told.

 

[drpotato]

Thanks. A lot of this is like Chinese to me but I’ll try to translate your steps. I’ve only got a couple extractions under my belt and I’m not afraid to admit that I was just following directions. I want to learn the science behind it but for now I’m just doing s I’m told.

the important part was, where i said dont literally do what i said, its just a simple description of the process, make sure to follow a tek as there are some extra bits that probably matter.

For the most part though you can literally just treat your extract you currently have as if it were bark, except now, your quantities of acid and base are strictly set by the amount of extract you have, rather than say, needing enough lye to cause the tannins to change color if thats how you are tracking things.

Important things to do to on crude extract doing a mini AB:

after you acidify it, and defat, filter it. dust and silt can cause emulsion. plus fats will probs get stuck in the filter. while dmt salt is unaffected.

Base with a gentle alkaline material like carbonate. lye is overkill here, and overbasing is undesirable. plus without any solids floating around, CO2 bubbles wont form foam/scum.

 

[WaffleStompN214]

the important part was, where i said dont literally do what i said, its just a simple description of the process, make sure to follow a tek as there are some extra bits that probably matter.

For the most part though you can literally just treat your extract you currently have as if it were bark, except now, your quantities of acid and base are strictly set by the amount of extract you have, rather than say, needing enough lye to cause the tannins to change color if thats how you are tracking things.

Important things to do to on crude extract doing a mini AB:

after you acidify it, and defat, filter it. dust and silt can cause emulsion. plus fats will probs get stuck in the filter. while dmt salt is unaffected.

Base with a gentle alkaline material like carbonate. lye is overkill here, and overbasing is undesirable. plus without any solids floating around, CO2 bubbles wont form foam/scum.

Gotcha. I got the carbonate. I also got hexanes & heptane and real lab equipment to use on the next one.

 

[WaffleStompN214]

no. because then you would need to neutralize the lye with vinegar, and then afterwards youd need to re-basify again. Granted, you *could* but, the molar mass of sodium hydroxide is 40g, while acetic acid is 60g, meaning it takes 3 parts by weight of pure acetic acid, to neutralize 2 parts sodium hydroxide. In 5% vinegar, and assuming acetic acid is exactly as dense as water, this works out for 5% of the stronger sort of cleaning vinegar, to require roughly 20x1.5 =30ml of cleaning vinegar to neutralize each gram of sodium hydroxide.
What you can do now though is run a mini AB on what you have. Im not sure how much vinegar to use but it wont be much really. dmt has a molar mass of 188g/Mol so, for every suspected gram of DMT there, you add 188/60 then times 20 for 5%, lets just call it 60ml vinegar. excess wont hurt so calculate it based on your expected best case scenario then add like 20-30% more or something. Otherwise, you should be able to tell using ph strips or a ph meter, the ph wont drop all the way down until the DMT is reacted, although it may take a little bit of time to actually react and do that. follow a tek for this not just what ive said, theres more to it.

I dont know who norman is or what their tek entails, they dont appear in the search engine, but, usually we start by acidifying the bark if we want to do a defat in the process. In a dry tek, which i assume is what this one is, we rely on a fairly pure source, and fairly good crystalization so that the crystals will form out of the fatty naptha, which you can then proceed to rinse away with additional cold naptha, to get acceptably pure spice, although the fats may themselves be solvating some DMT so while its an easy low effort method, the yield does suffer and the quality isnt as great as if the fat were omitted right from the outset.

Most teks balance yield, quality and complexity and sacrifice one for the other(s), MHRB generally contains nothing but DMT and trivial contaminants that are in low quantity and are easily removed.

On that note, take a ml of naptha and evaporate it on some glass and see if it leaves behind oil or not. you are supposed to check this anyway with your naptha source. its uncommon but it does happen.

I added vinegar solution (ph 4) to the goo but it’s not separating. I may just throw it away and start over. What, in your opinion, is the best tek for someone who knows nothing about chemistry to use? Are you in the US? I need to hire someone to give me extraction lessons viaFaceTime lol

 

[WaffleStompN214]

Know what, fuck it, I’m gonna start from scratch and hopefully not end up with goop this time.

 

[drpotato]

I added vinegar solution (ph 4) to the goo but it’s not separating. I may just throw it away and start over. What, in your opinion, is the best tek for someone who knows nothing about chemistry to use? Are you in the US? I need to hire someone to give me extraction lessons viaFaceTime lol

gums and such wont dissolve readily, dmt will. i hope you didnt actually discard that because the fact that it "wouldnt seperate" means that you had a definite seperation occuring and your solution was loading up with pretty pure dmt leaving junk behind.
and even then, you could have just added it all to your next batch of bark.

 

[barnaclebartley]

Possibly 400g powder gets
140g costic soda

 

[WaffleStompN214]

gums and such wont dissolve readily, dmt will. i hope you didnt actually discard that because the fact that it "wouldnt seperate" means that you had a definite seperation occuring and your solution was loading up with pretty pure dmt leaving junk behind.
and even then, you could have just added it all to your next batch of bark.

The next one is going to be in a different part of the country so transporting it there wouldn’t be worth it. I’m ready to start over with all the proper equipment this time. I’ve got bark, soda, carbonate, hexane, heltane, nap, and h20. Am I missing anything and what tek would you recommend for someone without a chemistry background but will still yield quality, regardless of amount?

 

[drpotato]

i mean, probs vinegar? if this bark produced too many byproducts maybe a quick'n'dirty method like STB isnt the way to go
it assumes your bark is pure to begin with, which it wont be if theyve added trunk bark for extra mass, it would also have some DMT too so its not like empty cutter, or just ground up the entire roots rather than just their bark, which at a certain scale is probably more convenient if you just have endless stumps you can process. Many convenient teks rely on the fact that DMT is almost the only naptha soluble thing m.hostillis ROOT bark that doesnt also stay in solution at super high concentration or freezing temps, i.e the only thing that crystalizes out when frozen or most of the solvent is allowed to evap away. STB on things other than MHRB require increasing levels of effort to yield a pure product.