Low yield on my 1st extraction, what went wrong?

[Jagube]

I'm doing my 1st extraction and here is what I did:

I cooked 100g of MHRB in water with a bit of vinegar twice, then froze and thawed the plant material and cooked it two times more. Then reduced it to 300ml.

I saved 1/4 of the tea for drinking and saved the remaining 3/4 (75g worth of rootbark) for the extraction.

The tea was quite active at 2g, so it wasn't bunk material or a dud tea, but probably less active than other MHRB teas I've had in the past.

I decided to use Cyb's salt tek on the tea saved for extraction, with the difference that I was doing it on the tea and not on plant material.

I poured the tea in a 700ml bottle and added 15g dissolved in water. At first I didn't have NaOH, so I put in 15g CaOH dissolved / suspended in water, and added 15g NaOH dissolved when that arrived in the mail. I topped it up with water to 650ml and added 50ml light naptha (lighter fluid).

I've done two pulls so far and they proceeded as follows:

* Warm the basic soup with naptha in a heat bath
* Shake / upturn the bottle several times over 30 - 60 mins
* Wait for the naptha to separate from the basic water
* Decant the naptha using a turkey baster and put it in a pyrex dish in the freezer
* Let it sit in the freezer for 18 hours
* Pour off the naptha and keep for re-use in subsequent pulls; dry the crystals with a cold fan

The crystals collected were very white, with very little impurities and minor stickyness. However, there was not much of them.

The 1st pull yielded 175g, the 2nd only 80mg, totalling 255mg. Of course I'm going to do more pulls, but I thought with the salt tek most of the DMT gets pulled in the first 2 - 3 pulls, so I'm not expecting much more. After the 2nd pull the total yield is 0.34%, so even if I do more pulls, I don't expect it to go above 0.5%.

Do you have any ideas on what I may have done wrong?
Could the soup be not basic enough? Does the CaOH interfere with the NaOH? Did I not make the soup warm enough for pulling? (It was really hard to warm it up in the heat bath as the bottle is tall and only the bottom 1/5 of it sits in the hot water.)

 

[downwardsfromzero]

Sounds like you haven't pulled all the goods yet. It seems as though the DMT can stick to calcium salts a bit (just a hunch, based on some observations... alternatively, calcium particulates adsorb naphtha somewhat, which then floats off only slowly.) If your naphtha isn't saturated enough it won't precipitate so well, especially if your freezer isn't as cold as it could be.

If you leave that base tea for a month or so, I'll bet that a bunch of DMT floats to the top. But adding a bit more NaOH and pulling again with (the same) naphtha, while making a better attempt at warming things up, should see your overall yield improving without the long wait - unless it's the calcium particulates clinging onto your naphtha.

How did the volume of your recovered naphtha pulls compare with the amount originally added?

 

[Jagube]

Thanks. Sure I haven't pulled all the goods yet, but it was my understanding that with the salt in the mix most of the goodies should be pulled in the first 2-3 pulls. I've seen someone report to have gotten goodies out at the 18th pull. But the steep decline of yield in my case (from 175mg to 80mg) doesn't look promising.

If your naphtha isn't saturated enough it won't precipitate so well, especially if your freezer isn't as cold as it could be.

I don't think my thermometers are very accurate as one measured -20C at setting 3, and another -16C at setting 6, which is supposedly the coldest. But even if we take the more pessimistic value of -16C, that should precipitate the DMT fairly well?

The naptha I pour off after freeze-precipitation is not clear, but cloudy, so perhaps the DMT is not precipitating as well as it should be, or could it be impurities? The cloudiness is white, not yellow or any other coloring.

If you leave that base tea for a month or so, I'll bet that a bunch of DMT floats to the top. But adding a bit more NaOH and pulling again with (the same) naphtha, while making a better attempt at warming things up, should see your overall yield improving without the long wait - unless it's the calcium particulates clinging onto your naphtha.

Will all more NaOH and try and warm things up better.

The mixture settles into three layers (from top to bottom - see attached photo): naptha, a clear(-ish) amber liquid, and a light-brown/grey suspension - presumably the undissolved CaOH. The naptha layer in the photo is thin as most of the naptha was pulled off.

If the calcium is trapping my naptha, I understand if I wait a month the DMT dissolved in the trapped naptha will float to the top naptha layer, but the trapped naptha will still stay at the grey bottom layer, so I'll have to add more naptha to recover it reasonably quickly?

How did the volume of your recovered naphtha pulls compare with the amount originally added?

I didn't measure it, and I'm not basting off all the naptha as the bottle's neck is fairly wide and I don't want any of the basic solution to get into the naptha. For my last pull I'll suck up all the naptha with a bit of basic tea, pour it into a narrow glass and try to recover more naptha.

Edit: I put the 2nd pull (after collecting the crystals) back in the freezer and after a few hours got another 60mg, bringing the yield from the 2nd pull from 80 to 140mg. So the freeze precipitation clearly wasn't complete or the crystals dissolved back into the naptha. Now after the 2 pulls the total yield has gone to 0.425%.
And the reason the thermometer was reading -16C was that it was on top of the pyrex. I put it flat on the bottom of the freezer compartment and the reading dropped to around -28C. Also the pyrex in the 2nd pull was sloping and not flat. I'm going to put it flat from now on, which should improve the efficiency of the freeze precipitation.

 

[Prima Materia]

Are you using light or heavy naptha ? I read that heavy naptha is not very good for freeze precipitation, while it is good to extract the goods. Light naptha on the other hand is not so efficient at extracting the spice, while it is good for freeze precipitation.

Light naptha vs heavy... - STB - Welcome to the DMT-Nexus

 

[Jagube]

I'm using lighter fluid, which is light naptha.

 

[downwardsfromzero]

I read that heavy naptha is not very good for freeze precipitation

IME it's the aromatics (toluene,xylene) content of naphtha that prevents freeze precipitation. Heavy (medium, maybe...) naphtha is a good solvent and freeze precipitates well, but you really have to dig into its technical details before use - and bear in mind that some kind of further purification is a must if using heavier naphtha.

Even if freeze precipitation doesn't work, an acid wash will recover the alkaloids from the NPS (eventually) to a more concentrated form which can then be re-extracted.

 

[Jagube]

The 3rd pull yielded 180mg - more than either of the first two (170mg and 160mg), so I'm up to 0.75% yield after 3 pulls and I feel there is more to come. Maybe not that terrible after all. And considering the first three yields are roughly equal, I suspect the naptha gets saturated and using more of it could have gotten that out in a smaller number of pulls. Too bad my bottle is already full.

The 3rd pull used more heat and more naptha, and some of the precipitate is yellow. I'm wondering if that's the famous yellow spice, or could it be that the basic solution got into the naptha and some nasties (NaOH?) crashed out?

Also is it best to pull while the solution is hot (because hot naptha holds more goodies), or is it that once the goodies are in the naptha, they stay there until frozen out of it?

 

[downwardsfromzero]

Hot pulls more. Yellow spice is quite normal with higher temps. You'd see dark blobs if there was base soup contamination.

 

[Jagube]

Hot pulls more.

Thanks, but I wonder if the solvent subsequently loses spice as it cools down to room temperature, or keeps all it has absorbed?

The yield after 4 pulls is 1.05%, I guess I'll do a couple more pulls and stop at that. My next extraction will probably be on 100g and on plant material as in Cyb's Max Ion tek.

I tried 30mg of this first extracted spice orally dissolved in vinegar with harmalas and it was a very different to the plant teas I've had.

 

[Jagube]

For the sake of completeness I'd like to add that after 6 (?) pulls the yield got up to 1.425%. At that point I decided to stop pulling with naphtha and switch to vegetable oil in the hope that this yields a fuller spectrum product.

 

[Prima Materia]

I read that heavy naptha is not very good for freeze precipitation

IME it's the aromatics (toluene,xylene) content of naphtha that prevents freeze precipitation. Heavy (medium, maybe...) naphtha is a good solvent and freeze precipitates well, but you really have to dig into its technical details before use - and bear in mind that some kind of further purification is a must if using heavier naphtha.

Even if freeze precipitation doesn't work, an acid wash will recover the alkaloids from the NPS (eventually) to a more concentrated form which can then be re-extracted.

Thank you for pointing this out.

I'm in the process of performing a DMT extraction right now. Since I'm using heavy naphtha and was not quite sure about it's eficiency I did some more research and talked with some members about it which gave me the same information.

This is the naphtha I have right now: Hydrocarbons, C10-C13, isoalkanes, cyclics, < 2% aromatics --> on the heavy side.

I'm aware of it's problems that are: very slow evaporation and the problem of probably not evaporating completely from the crystal mass.

It seems to pull DMT well from my basic solution and it seems to freeze precipitate well --> on the label it says that it contains less than 2% aromatics which explains why the freeze precipitation works.

downwardsfromzero --> What kind of further purification would you suggest ? You mentioned the acid wash and then extracting again - in that case on should indeed use a different solvent like light naphtha and recrystalise or small quantites of toulene, xylene and evaporate ?

 

[downwardsfromzero]

downwardsfromzero --> What kind of further purification would you suggest ? You mentioned the acid wash and then extracting again - in that case on should indeed use a different solvent like light naphtha and recrystalise or small quantites of toulene, xylene and evaporate ?

Simple evaporation of any lighter solvent would still leave the heavy residue around the crystals, so you'd need to do either a mini A/B or a recrystallisation, again using a clean-evaporating solvent for either of these processes.

And there's always FASA, of course.

All of these methods are described in the forum or the wiki - but, briefly, recrystallisation from warm heptane or light naphtha is most straightforward.

Using a water bath, warm your solvent of choice to about 50 C and, with your DMT in a separate small container, add the minimum of solvent such that the DMT is all dissolved (it will most likely melt at this temperature). Cover the vessel containing the DMT solution and allow it to cool slowly, first at room temperature, then in the fridge and finally in the freezer. Remove the solvent and recover the crystals, being sure that the remaining solvent has been allowed both to drain off and evaporate from the crystals. Keep the vessel closed when it is still cold otherwise condensation will form.