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First Timer w/ some q's

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LeRenard

LeRenard

Rising Star
Hello,

I'm about to begin my first MHRB extraction and have some questions for you fellow trippers.

1. I would prefer not heating the acid soaks. Is 7% acetic (pH 3, I think) strong enough ? And if so, how many hours should I let it soak (at room temp) ?

2. I got access to NaHSO4. Would this work, instead of vinegar ? I could get my pH 2 right and avoid heating. I have heard of extractions made with muratic or chloridric acid, but never with sulfuric acid.

3. I would use heptane (bestine) as a NP solvant. Is there anything different between using naphta and heptane (quantity, methods, etc.) ?

4. Is it true that ammonia used for washing spice (if necessary) can be put back in acid water and re-extracted ?

5. Is there any alternative to lye for basifying ? I want my spice to be as clean and smooth as possible.

6. When heating solvent in sealed mason jar, would the pressure get too high and make it pop ? How much solvent can I heat at once this way ?

Thanks in advance,

Le Renard
 
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LeRenard said:
Hello,


4. Is it true that ammonia used for washing spice (if necessary) can be put back in acid water and re-extracted ?
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This better not be true. The whole point is that impurities are supposed to be soluble in ammonia, but not the DMT itself.


LeRenard said:
6. When heating solvent in sealed mason jar, would the pressure get too high and make it pop ? How much solvent can I heat at once this way ?
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Definitely possible. SWIY should definitely periodically release pressue from the jar (open it) so it doesn't explode.
 
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I truly dont know the precise chemical reactions that take place when doing an ammonia wash. I am sure that DMT desolves in acid. I am also sure that ammonia is basic. I also know that you loose somwhere approaching 10% of your spice when doing an ammonia wash. I presumed that tiny bits of spice wash through the coffee filter pores with the ammonia as it carries out the other impurities. With that it mind I feel it would be verging on the criminal not to re-extract the spice in your next pull.

I think ammonia washing is a real cool thing to do. It's simple cheap and effective but why sit back and say fine, I'll write of that 10%. Its a no brainer for me.
 
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Lye is a fine base to use. Lye isnt even soluble in heptane so its probaly wont get in your spice anyway. plus you can always do a wash with pH 8.5 water and sodium carbonate to remove any from your organic solvent.

The acid people i dont know always use acetic acid glacial. But not everyone has that so HCl would work but you cant reduce your water volume really otherwise it will concentrate the acid. No one I know used sulfuric acid but i dont see why it wouldnt work. pH 3 is a fine pH to work with. If your not using heat soak for day or two per extraction. Id recommend at least 3 acid water pulls.

Heptane is fine. The only difference between heptane and hexane is one carbon longer on the chain.

People I dont really know never use ammonia wash so i dunno about that.

If your doing acid base exctaction I dont know why you would heat it in a sealed jar. Acid base you dont need heat when your defatting or when you are taking you spice out of basic solution. maybe it helps with yield though?? id imagine it helps with solubility but in that case i would just add warm heptane and collect it after a few gentle shakes and emulsions settle.
 
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burnt said:
If your doing acid base exctaction I dont know why you would heat it in a sealed jar. Acid base you dont need heat when your defatting or when you are taking you spice out of basic solution. maybe it helps with yield though?? id imagine it helps with solubility but in that case i would just add warm heptane and collect it after a few gentle shakes and emulsions settle.
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You must heat the solvent when re-crystallizing.
 
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I heard SWIM lets the bark soak for 8-12 hours @ pH 2. If I do it @ pH 3, shouldn't I let it soak like, 10x longer ? 80 hours minimum ? 2 soaks takes a week.

I have two options : 1. Use phosphoric acid (easy to find, high yield). There seems to be little or no litterature on using sulfuric acid solution/salt.
2. Use pH 3 vinegar and heat it. Is it wrong to do acid cook @ pH 3, or do I definatly need to dilute ? Would it increase yield ?

Already have vinegar, but the odds are I'd go with phosphoric acid. Having a hard time finding lye. When I ask for heptane/toluene/lye over the phone I always get lazy negative answers. I think I'll have to see by myself.

Is there something wrong with using pre-diluted causic soda solution (maybe concentrate) ? I heard it allows lye to follow solvent more easily.
 
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if it is your first time they stright lye extract on erowid is pretty foolproof it yeilds nice white powder and is really easy swim has been pulling at least 5 grams per kilo more if you keep reusing the naptha but as you wieght goes up it starts to get more yellow either way if you want simple so you can familerize yourself with the basics that is what I recomend
 
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hoff1943 said:
if it is your first time they stright lye extract on erowid is pretty foolproof it yeilds nice white powder and is really easy swim has been pulling at least 5 grams per kilo more if you keep reusing the naptha but as you wieght goes up it starts to get more yellow either way if you want simple so you can familerize yourself with the basics that is what I recomend
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It's not that simple, and old. I don't want anything foolproof, I want my own ultimate tech, that fits chemicals I have access to. Can you answer at least one of my questions ?
 
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Great questions .. ! And Woo Hooo ! An enthusiast who want to do it 'properly' by solubilizing teh dmt in water first ! Why take a 'short-cut' to make an impure product you have to wash..?

Just use the required and called-for reagents, skip the sulfuric acid for now. Get HCL, it is available in pool supply stores. Phosphoric acid was talked about here too, and folks were saying the mineral acid you use does affecet some qualities of the product. Acetic acid is used too, but at pH 3 - 4 it's likley you'll need to extract for longer and/or cook it.

Heat is not a problem - it's just more work. Stirring the acid soak fo r3 hours at 55 deg C (pH 2 soak) is probabaly the equivalent of 12 hours at room temp, but you must stir it as often as possible to be thorough.

Filter well ! this may take 8 hours too, to drip through a tight milipore-sized filter. You get clean, clear deep purple dmt-ful-solution then !

In the end, if yeild is less than 0.7% and you used good quality MHRB, then you may have to improve the tek. I say acid soak at pH 2, basify to pH 11.5

Surely you know to pulverize the MHRB first - grind the shit out of it, that opens it up to easy access by the H+ in the acid water.

Soaking at a pH of 2.0 at room temp for 8 hours gets 75% of the dmt out - there's a big yeild if you process the first acid extract all the way to evap'. Just shake the jug really hard very often during each acid-soak.

The second soak at RT for 8 hours at pH 2.0 gets the last 25% out, almost entirely cleaning the MHRB of dmt. It's not worth extracting a third time, but perhaps leave it for a week or more, shaking the shit of of it and you'll find another 1-2% might be salvagable.

Other people recommend 'pulp-milling' the remaining MHRB in an STB tek - you can probabaly get another 5% after doing the A-B method, they say.
 
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Here's my tek (summarized).

1º Put 1 lb ground bark in 1l HCl solution (pH 2).

2º Wait 8 hours (shaking often). remove liquid and put to fridge. Repeat 1 & 2.

3º Combine liquids and filter through t-shirt (decent enough?).

4º Put 250 ml heptane in jug, make pH 11.2-11.5 with NaOH (shaking). Can I use pre-diluted NaOH concentrate/solution, instead ?

5º Shake 5 minutes, then wait 4 hours, and remove heptane layer with a turkey baster. Repeat 4 & 5 twice, with twice solvant for the last time.

6º Combine and CFC.

Something wrong ? I also plan to extract dark spice.
 
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To address some of your questions from this last post:

Q1. Is the decant enough, rather than a full filtration?
A1. Yes, assuming you are good enough at decanting to remove the solid matter. Otherwise, do a filtration. Point being: remove all solids.

Q2. Can one use pre-dilute NaOH solution?
A2. You can use NaOH that has already been dissolved into water, yes. As long as you bring the pH to ~11, it doesnt really matter.
 
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While I don't consider myself a natural product isolation chemist, I really do not see the point in the initial acidification step. Why not simply perform a basic extraction into organic solvents, get the product, and do a crystallization purification? It just seems like you would be more likely to loose material with the extra steps. Additionally, exposing tryptamine alkaloids to acidic conditions will invoke pictet-spengler reactions, forming beta-carboline by products out of the desired compounds.

However, this is coming from someone who typically makes molecules in RB's rather than extracting them from plants. In my working with certain tryptamines, I typically avoid acidic conditions..otherwise the red colored carbolines prevail...

To read about pictet-spengler reaction (which is a pretty sweet mechanism) check out Pictet–Spengler reaction - Wikipedia
 
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rbwoodward said:
To address some of your questions from this last post:

Q1. Is the decant enough, rather than a full filtration?
A1. Yes, assuming you are good enough at decanting to remove the solid matter. Otherwise, do a filtration. Point being: remove all solids.
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I was asking if filtering through a t-shirt was decent enough, el ka bong suggested a lab filter.

rbwoodward said:
To address some of your questions from this last post:
It just seems like you would be more likely to loose material with the extra steps. Additionally, exposing tryptamine alkaloids to acidic conditions will invoke pictet-spengler reactions, forming beta-carboline by products out of the desired compounds.
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Why would there be any aldehydes in the solution ?
Straight to base teks require an enormous lye quantity, makes purification harder and brings the need to wash, which we don't want. And for idiots who claim that "lye isn't soluble in naphta", well think about it harder and you'll discover that dmt molecules are surrounded by water molecules. The more the pH, the more lye that passes through, as simple as that.
By doing several pulls, there is little or no loss with acid/base teks ; certified great yield.
The only pro to stb's is speed. Who cares. It's not like I need to extract once a week.

I want my final product as clean as possible. I want 'smooth' smoke. If spice 'burns', on first smoking attempt, I will wash. Can someone explain exactly how to wash with soda ? Or has anyone heard of cleaning with vodka/alcohol ?
 
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I do not see the problems with purity when using a STB extraction. I do not know of any specific artifacts that could be formed from these conditions especially if you are using naptha and hexane or toluene solvents, which tend to be very inert and are nice for avoiding unwanted artifacts (the same does not go for chloronated hydrocarbons!).

rbwoodward interesting reaction could play a role in artifact formation of acid extracts. however the conditions in an acidic solution of m. hostilis (unless at low low pH and high heat) may not be enough to provoke a large number of such reactions. i dunno for sure but id imagine people would be detecting such artifacts more often if that was the case ( maybe they are i dunno havent looked into it).

Doing a wash to remove residual lye or basic solution from your organic layer is very simple. just take sodium carbonate make pH 8.5, (if its a little higher it wont matter) solution and pour it through your organic layer one or two times. just do this step quickly as emulsions would be minimal. people i sort of know doing these extractions have never had spice that burned or bothered ones throat never even made them cough. sometimes theres a small wheeze after everything is over but thats about it.

also i wouldn't call someone an idiot for saying NaOH isn't soluble in hexane or naptha or what not. solubility is a very relative term. try making coffee with cold water at normal atmospheric pressure not much is going to happen. put it too 100 degrees and all types of chemicals dissolve in it. put dmt in cold hexane not much is going to happen. water boils at 100 degree C but will evaporate at room temperature. sorry im baked and rambling again...oh yea but i wanted to say dont clean with alcohol dmt is soluble (haha that word again) in methanol and would also be soluble (haha that word again) in ethanol.
 
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burnt said:
also i wouldn't call someone an idiot for saying NaOH isn't soluble in hexane or naptha or what not. solubility is a very relative term. try making coffee with cold water at normal atmospheric pressure not much is going to happen. put it too 100 degrees and all types of chemicals dissolve in it. put dmt in cold hexane not much is going to happen. water boils at 100 degree C but will evaporate at room temperature. sorry im baked and rambling again...oh yea but i wanted to say dont clean with alcohol dmt is soluble (haha that word again) in methanol and would also be soluble (haha that word again) in ethanol.
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The point ? Solution will be hot, when extracted (so will the hexane).
The thing is : I DON'T care about artifacts, I care about lye. Even with 'inert' solvents, you carry lye, because water follows organic components, such as DMT. The amount of lye involved in making water pH 11.2 and pH 14+ is a thousand times. A/B's assures high yield. You only lose spice when hexane pulling, just as in a STB tek.
And thanks for the washing tip.
 
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It is absurd to think you cant get clean product through a purely basic extraction. Recrystallization being the final step - thats as clean as it comes (with or without chromatography in most cases) for work at this level, regardless of how much lye you use.
 
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