Mini A/B assistance please

[Wombling Free]

Hello,

I've had success with a STB extraction on 100g MHRB, collecting 1.65g crude product after 4x naphtha pulls and freeze precipitating.

I recrystallised the product x3 with heptane, reducing quantity down 1.52g > 1.30g > 1.20g. From the second Re-X (1.30g) absolutely everything dissolved in 45ml solvent, no residues left in the beaker. I needn't have bothered with the third, was simply a repeat and slight loss.

From that point it seems fairly clean and easy to scrape up to weigh (no goo), unlike the naphtha or first Re-X results.

Before I go on I've read the "..Enough GOO questions! read this.." thread, I suspect what I have is perfectly active and able to be vaporised. But I was after white crystals and have attained some albeit in tiny quantity .

So, yet again I dissolve my pale yellow DMT in fresh warm heptane, 35ml to start but I use extra to ensure virtually nothing remains in beaker, it's walls were still coated on first emptying.

This solvent I pour into a bottle of acidic solution pH 3 and shake at room temperature. The previously saturated/cloudy solvent appears clear following separation (in bottle). The acidic solution also appears white for a long while post shaking but returns to water-like eventually.

The removal of solvent, basifiying, pulling with clean solvent etc, etc is carried out and my final result is a measly 0.3g, try not to LOL. Was there really that much plant oils/fats still making up the weight?

What I'm trying to ask (for better result) is whether or not I should heat the acidic/solvent mix before separating?
Should separation be done quickly after shaking while it is still white?
I had let it sit a good while before doing so.
Does the DMT work its way back to solvent when left? The pH 3 hadn't changed before basifiying
> pH 12+.

I'll attach a few images if I can (1000 words ), I take a lot!
Thanks for reading, viewing.

 

[blue.magic]

Here is an advice from pete666 from out correspondence:

Well, because we titrate, we know how much dmt fb was salted. The salted water is reduced. NaOH is added. I don't measure anything, just add enough. More NaOH won't hurt anything.
So when we have super cloudy basified water + dmt fb, we can add heptane - about 20ml/g of dmt fb. Then we heat it up to about 60C and mix thorougly. Heptane gets colored. I do it in erlenmeyer flask. Once mixed, I use 50ml pipette to remove heptane and pour it into beaker. The pipette is heated by clean hot heptane beforehand, so dmt won't precipitate in it. The beaker with heptane is left to cool down to room temp slowly, then put into fridge, then into freezer. The yellow precipitate first, dmt later. After removed from freezer and dried 12h with airflow I use knife to scrape just the white crystals, not the yellow. It is easy, as yellow has different structure. Yellow stays in the beaker for next heptane pull.
I repeat the same process with less heptane (next pull). The same beaker with yellow residue is used, so all the yellow from all pulls stays in one beaker. After freeze-precip you know how much the solution was saturated. The crystals in the beaker tell you tell you whether to do next pull.
The yellow residue can be re-x'ed as much as desired. I usually leave half of the yield in the white and half in the yellow. The yellow is broken up by knife and dried with air-flow over few days, with ocassional crushing. The result is dry yellow powder.

The color of (properly basified, rather more than less) basic water with dmt fb tells you when to stop too. You simply don't see any dmt in it

 

[Wombling Free]

Thanks for your reply blue.magic.
I had in fact just a short while before posting seen some of your results in a thread started by KloudQ7, "Crystals everywhere! My pics". Those Tetrahydroharmine hydrochloride images are exceptional!

Perhaps I shouldn't have included the shot of the crystal lake (as I like to call it), all the suspended DMT dissolves once I add a bit of heat to the bottle, there is just so little of it

After shaking the warm bottle, I top it up with an excess of the same NaOH solution used to basify (also warm) to bring the solvent right up into the narrow neck for easy pipetting to freeze precipitation dish, avoiding any emulsion. I had done the same previously with acidic solution/salted water except the solvent goes back into storage jar. I thought this was quite a good technique but Pete666 talks about reducing the salted water, I have done the opposite, is this a problem?

I think I understand what he says about separating white DMT from yellow precipitate, I have an image which may indicate this. Taken before mini-A/B attempt, left 3 hours at room temperature. But I hadn't thought it would separate cleanly (different structure described) so continued Re-X'ing. In future perhaps I'll just pour off the heptane and do the same? Although it still looks a bit tricky to me. Ok, now some images of these things.


1. As described last, Re-X beaker with fairly white DMT sat above yellow plant fats.

2&3. Crystalline pale yellow DMT on dish, naturally spread after solvent removal, dry, then scrapped up.

Then the mini A/B
4. Acidic/salted solution

5,6&7. Basified, very little NaOH solution used 30ml @pH 12.0. Solution is stirred and measured as pH 12.7, not sure why it increases?

8. I split the solution, roughly half returned to bottle.

9&10. Hot Water bath before shaking and top-up from beaker, using a separate pure NaOH solution.

11. Solvent fully removed.

Into freezer @-25°C, 24 hrs.

Process repeated (after basifying) 4x (2x each bottle) and the overall weight was still only 0.3g, basically nothing on the 2nd run.
After the multiple Re-X'ings I had hoped for over half a gram, at least.
Nothing has been disposed of, but is it even worth another go?
Is some of the DMT still in the solvent mixed with the acid @room temp/cold, should I heat it?
Any other major mistakes made?
Thank you.

 

[pete666]

I recrystallised the product x3 with heptane, reducing quantity down 1.52g > 1.30g > 1.20g. From the second Re-X (1.30g) absolutely everything dissolved in 45ml solvent, no residues left in the beaker. I needn't have bothered with the third, was simply a repeat and slight loss.

I would do mini A/B before re-x. If you HCl titrate your non-polar solvent, you know how much dmt you have and you can use the solvent immediately for next pull. The knowledge is important, because you know where you are and what to expect in next steps. If you get less, you know you left something behind. And when you have your salted water as a result, you know how much hot heptane use for subsequent pulling.

So, yet again I dissolve my pale yellow DMT in fresh warm heptane, 35ml to start but I use extra to ensure virtually nothing remains in beaker, it's walls were still coated on first emptying.

This solvent I pour into a bottle of acidic solution pH 3 and shake at room temperature. The previously saturated/cloudy solvent appears clear following separation (in bottle). The acidic solution also appears white for a long while post shaking but returns to water-like eventually.

I suggest HCl titration, so you know how much dmt was transfered. If you need to know how much HCl is for dmt, just let me know. I have excel calculator for this.

Hello,

The removal of solvent, basifiying, pulling with clean solvent etc, etc is carried out and my final result is a measly 0.3g, try not to LOL. Was there really that much plant oils/fats still making up the weight?

If you did HCl titration and now got just so little, you could be sure the mistake was in the last step. I already did a mistake and added too little hydroxide in this step. Fortunately I realized it and could get everything out eventually.

What I'm trying to ask (for better result) is whether or not I should heat the acidic/solvent mix before separating?

Heating helps to fight the emulsion and helps to transfer dmt faster. Anyway, if you shake properly and long enough and don't have problems with emulsion, there is no need to heat up.
Again, use titration and you will be sure everything is transfered.

Should separation be done quickly after shaking while it is still white?
I had let it sit a good while before doing so.

No, you want to ensure freebase is converted to salted and dissolved in water. No hurry

Does the DMT work its way back to solvent when left? The pH 3 hadn't changed before basifiying
> pH 12+.

Dmt stays in its salted form when pH<7. It is soluble in water at that pH. It is soluble in non-polar only when basic (pH>7). Check the calculator so you have an idea what is happening.

The most important message is ... try to stay informed what is happening within the extraction process. HCl Titration is really simple and helps a lot. Once you have few successfull extrations in your pocket, you might skip it, but if you are not sure and want to diagnose what's wrong, it is priceless.

 

[Wombling Free]

Thank you for the advice and useful links pete666, I have another 200g material to work with, will probably split it in half and use HCl titration on my next go.

One thing I hadn't said was that I'd used phosphoric acid 85%, diluted in distilled water.

Fortunately I had ordered litre sized quantities of both sulphuric and hydrochloric acid 98% and 37% respectively.
That, before foolish people started throwing it at each other making it unavailable to the general public without documentation

Talking of emulsion, there was virtually nil with the mini A/B but in my thicker STB soup there had been.
But I'd written some notes on my technique of clearing it (worked for me at least) so will post those shortly with a set of pictures, might help some folks.

Could be a while before I begin a new extraction and this time I'll A/B it from the start but will update here when I put into practice what you've shared :thumb_up:

 

[pete666]

Just one note. I am using titration with toluene, because I use it for initial pulls. Toluene is not miscible with water. Naphtha should not be as well, but my experience is heptane(part of naptha) used for many freeze-precips left traces of NaOH when evaped. This leads to conclusion there had to be some water within heptane. And any NaOH in naptha(in fact in water mixed with naptha) could make the titration useless. It would salt the result without prob, but the estimate of dmt content would be false(because of necessity to neutralize NaOH by HCl). I suggest using toluene or if naptha, I would test titration of naptha after mixing with water with NaOH without dmt. If titration reads 0mg alkaloids, it is safe.
Maybe someone else has experience with titration of naptha?

 

[Wombling Free]

Not quite the same but I had done a quick test to see if anything would freeze precipitate when heptane solvent was shaken with a mixed solution of phosphoric acid and NaOH, thought perhaps trisodium phosphate? Phosphoric (the small amount used) stays water-like diluted but NaOH left a while always seems to leave a thin layer on the bottom of beaker/vessel. Over saturated perhaps?

There is also the same clouding I noticed when combining liquids with or without DMT present. I did it first on DMT containing solution and was :shock: thinking woah, that looks a lot! Not the case though as test (no DMT) produced the same, image of that above. Basified, but not all of it what we want, shame.

A non-DMT sediment settles in the mixing bottle when left.

Anyway, fortunately, dish out of freezer and time to dry left no contaminants as far as I could see. The n-Heptane used is 99.5% ACS, from a more affordable supplier but not Fisher(Scientific)-Price
Not sure why we've had different results regarding this solvent?
I had read here about sodium carbonate washes to remove NaOH and clean product. Don't know how effective that is though?

 

[pete666]

I am not sure we are talking about the same thing. There is no need to do sodium carbonate wash to get the final result without NaOH, as the tiny amount of NaOH dissolved in water mixed with heptane will stay dissolved when doing freeze-precip. As the liquid(heptane) is poured off, the result is lye-free, no worry.
I was talking about false reading of dmt amount within the pulled non-polar solvent caused by HCl necessary not to salt dmt, but to neutralize NaOH. Titration has to be precise, so the aim is to have the non-polar lye-free. If you don't get what I am talking about, please read and understand this first.