A/B Extraction , yet i failed again

[DefNotAnEntity]

hi Folks,

I tried extracting DMT once and i failed : DMT extraction - what mistake did i make
I tried again using different method.

I took 125g of Mimosa Hostilis Root Bark and grinded it to fine powder in a thermomix. Then i bathed the root bark in 50ml of apple avinegar acid and added 500ml of water.
Simmered for 2 hours.
Then i used nut bag and pressed the "DMT water" against it.
I added apple avinegar acidof acid and 500ml of water, simmered 2 hours and pressed it thru nut bag
Did the last round of 25ml of apple avinegar acid and 250ml of water.

I added 30g of sodium hydroxide, dissolved in some water. Added it to the "DMT water"

Then i added 125ml of heptan. Heat up the jar and was shaking it for a couple of minutes. I let it settle and after 1 hour i pulled i collected the heptane.

https://imgur.com/a/3NWBU5Q

I only collected 200mg of DMT out of 125g of bark. I should be g etting like a gram or even more.

What did i do wront this time? I put the effort and tried to follow every step correctly.
Please someone advise me

 

[modern]

The problem could be your bark material is weak... recently I've only been seeing outer root bark for sale here in Brasil and the yeild is around .3%.

Another issue is you only did a single pull try multiple water pulls and reduce the volume or go straight to base.

Try using less heptane. Do 50 ml pulls since you are getting low yield it'll be more saturated and lead to more precipitating form the heptane rathar than remaining soluble. Do a MINI A/B on the heptane with vinegar to pull the dmt seperate the heptane. Then add lye and only add back a lower amount of heptane.

 

[Transform]

Mostly what @modern just said. Add a bit more NaOH and do more heptane pulls. If you re-use the same heptane, it's now saturated and you won't have to do the vinegar backsalt (mini A/B) until the very end.

Aso, check that your freezer is as cold as possible to squeeze out a bit more yield.

What you have so far looks really nice!

 

[BongWizard]

I'll start by saying that you've got some fine looking spice there, despite the low yield.

I'd suggest not diluting your vinegar, and just use standard white vinegar if you insist on using vinegar at all (the chemist in me is screaming "just use 0.1N HCl"), apple cider is less acidic.

Do multiple non polar pulls with multiple mixings per pull and a warm pull to finish, collect the product in separate containers, freeze precip, before pooling for the final evap.

You can also try basing your bark soup and pulling directly off that (don't filter, just whack some NPS on top of the now based soup and carefully do a pull, evap in a separate container) to maximise yield.

You may also have bark that is older or harvested mature. I've seen yields vary between about 0.5% and 4% using the same method. Starting material quality is VERY important.

 

[Bas Sarkin]

-It looks like more then 200mg. Check if your scale is correct.

-Scrape it totally clean, for example with a credit card, that will increase the yield a little.

-A single shake-session+1 hour is a bit short. I do six hours of swirl sessions before I take the naphtha. I add the naphtha, mark the line between the solvent and the water, swirl it, then let it sit till the line is there again (to make sure nothing of the solvent is still hanging around in the water).

-Also dont shake violently, but swirl, so the layers will separate with ease in a few minutes, then swirl again for a couple of hours.

-Do several pulls with naphtha, till it does not yield anything anymore, 3 at least.

-Did you use freeze precipitation?

-Use as little naphtha as possible. Rule of thumb is: naphtha at room temperature will hold 30mg/ml, in -20 Celsius freezer it will hold 1mg/ml. So there is still 150mg in your 150ml of naphtha at freeze temperature. (you can get it by evaporating the naphtha). If you expect a yield up to 1500 mg, only use up 50ml naphtha for the first pull, even less for the next ones.

 

[DefNotAnEntity]

-It looks like more then 200mg. Check if your scale is correct.

-Scrape it totally clean, for example with a credit card, that will increase the yield a little.

-A single shake-session+1 hour is a bit short. I do six hours of swirl sessions before I take the naphtha. I add the naphtha, mark the line between the solvent and the water, swirl it, then let it sit till the line is there again (to make sure nothing of the solvent is still hanging around in the water).

-Also dont shake violently, but swirl, so the layers will separate with ease in a few minutes, then swirl again for a couple of hours.

-Do several pulls with naphtha, till it does not yield anything anymore, 3 at least.

-Did you use freeze precipitation?

-Use as little naphtha as possible. Rule of thumb is: naphtha at room temperature will hold 30mg/ml, in -20 Celsius freezer it will hold 1mg/ml. So there is still 150mg in your 150ml of naphtha at freeze temperature. (you can get it by evaporating the naphtha). If you expect a yield up to 1500 mg, only use up 50ml naphtha for the first pull, even less for the next ones.

Hello,

first of all thank you for your response. I did freeze precipation.
I checked the scale unit. I had incorrect units set. It wasn't grams. LOL. I had 0.02 OZ which i thought is 0.2 g, but apparently is ~~0,6g.

When you mention swirling, do you have a device for it or you do it manually? I Mean you keep swirling, then waiting, then swirling then waiting for like 5-6 hours:?
Do I need to fill up the jar completely to avoid emulsion? If i use less naphta , there will be some more empty space in the jar.

Also shall I warm up the remainder before i swirl it? I kept in a room temperateure so its around 20C. Will it spoil/ go rotten over time? or is it safe to keep harvesting it for a aweek or more?

 

[Transform]

I checked the scale unit. I had incorrect units set. It wasn't grams. LOL. I had 0.02 OZ which i thought is 0.2 g, but apparently is ~~0,6g.

@Bas Sarkin was right on the money there. 1 ounce [avoirdupois] = 28.4 grams (unless it's a troy ounce, which is often used for gems and jewellery - then your yield will be even better, with 1 ounce troy equalling 31.1035 grams. Check your scale's specification for clarification). You're looking at a good 550 to 600mg either way.

 

[Transform]

When you mention swirling, do you have a device for it or you do it manually? I Mean you keep swirling, then waiting, then swirling then waiting for like 5-6 hours:?

Inferring from what Bas' reply says, it sounds like manual swirling to me:

I do six hours of swirl sessions before I take the naphtha. I add the naphtha, mark the line between the solvent and the water, swirl it, then let it sit till the line is there again (to make sure nothing of the solvent is still hanging around in the water).

A sort of rocking, rolling, 'pedalling' action helps maximise the contact area between the two phases without breaking them up into small droplets.

It's possible to do other things while waiting for the naphtha to separate. I'm inclined to think that six hours is a very generous amount of time for this process, and it will probably rather shorter for an A/B extraction than a more sludgy and viscous STB.

Do I need to fill up the jar completely to avoid emulsion? If i use less naphta , there will be some more empty space in the jar.

It shouldn't be an issue if you're not shaking the jar vigorously, but you can always top up with water (or brine) if it bothers you, or if you prefer to shake the jar.