2nd time extracting produced worse yields

[dazultra]

Hi Folks,
My first try was with 50g of Acacia Acuminata root bark; I did a cold extraction with heptane using 24-hour soaks at each stage, only doing one pull and got 176mg.
This is what I followed

https://www.reddit.com/r/DMT/comments/9qsyda/acacia_acuminata_extraction_notes

This time, I followed the same process but used a heat bath and naphtha (Shellite). I performed three heated extractions and three pulls with naphtha. I also washed the naphtha pulls in water. I was excited because I thought all the extra effort would produce a win. This morning, I checked my results, and they were even worse, at a measly 128mg.

I have some questions.

Can the bath temperature be too high? I bought a cheap electric heater, and its lowest temperature is 60 degrees. The water never got to a bubble simmer heat but was very warm to the touch. I would say it was probably 60 degrees. Is there an optimal temperature? Should I have had it lower or higher?

Is heptane a better fuel? Should I stick with that? My results last time were cleaner looking. I'm in Australia and heard that the Naptha sold here isn't as good as it used to be (I'm using Diggers Shellite)

My bark and vinegar pH was 3, maybe 4; when I added salt and NaOH, it went to 14. Are these correct?

Is there a better tek I should follow for this kind of bark?

I really appreciate any help you can provide.
Thanks!

 

[Phenethylamine23]

Just to clarify, you did three pulls with warm shellite and freeze precipitated?
How much shellite did you use?

Australian shellite has poor carry capacity from what I've heard.

Temperature is good, close to boiling allows solvents to carry more than when cold

 

[dazultra]

Just to clarify, you did three pulls with warm shellite and freeze precipitated?
How much shellite did you use?

Australian shellite has poor carry capacity from what I've heard.

Temperature is good, close to boiling allows solvents to carry more than when cold

Yes, three. I pulled with warm shellite 100ml each time, 400ml total (I remember now that I did it four times), and froze after. I also heated the vinegar and bark and strained three times at the start.
Do you think the temperature was too low? Should I have aimed for more of a boiling simmer? I could put my hand into the water, and it was fine, like a very warm bath.

I can use heptane again, Zippo lighter fluid, or Xylene. Which would you recommend?

Thanks for your help!

 

[Phenethylamine23]

How many pulls with water did you do on the bark? More the better until it starts to become less concentrated in colour, then you know you've extracted most if the water solubles.

Heat helps but can extract water solubles cold aswell, it just probably take more water. Heat help solvents carry more. More heat means can fit more into same volume of solvent.

The choice of non polar solvent depends on many factors, such If you want to freeze precipitate then heptane or shellite/naptha. If you dont mind the extra steps of salting out, extracting with xylene or dlimonene would be the go.

 

[dazultra]

How many pulls with water did you do on the bark? More the better until it starts to become less concentrated in colour, then you know you've extracted most if the water solubles.

Heat helps but can extract water solubles cold aswell, it just probably take more water. Heat help solvents carry more. More heat means can fit more into same volume of solvent.

The choice of non polar solvent depends on many factors, such If you want to freeze precipitate then heptane or shellite/naptha. If you dont mind the extra steps of salting out, extracting with xylene or dlimonene would be the go.

I did three pulls on the bark with just water and vinegar. The first pull was with 200ml of water, but I thought it was too little water, so I used 500ml for the second and third pulls.
What is salting out with xylene or dlimonene, how do I do that? Do I still freeze precipitate if I use those solvents?

Thanks!

 

[Phenethylamine23]

Cant freeze precipitate from heavier solvents such as dlimonene or xylene.
Can use them to salt out, meaning after extraction of basified liquid, seperate the solvent and wash it with an acidic solution (vinegar) to convert the alkaloid back into salt form therefore water soluble again. In essence it is a defat step aswell as oils will remain in the non polar region. After 3 x or more extractions of non polar solvent into vinegar can seperate it and evaporate the vinegar and be left with jim jam red goo. From there you have concentrated salt form alkaloids can refine further. Either do a dry tech converstion back to freebase and extract with acetone, or a variety of paths from there. You wont be left with cystals but can make changa or eliquid, or pharmahuasca.

 

[dazultra]

Cant freeze precipitate from heavier solvents such as dlimonene or xylene.
Can use them to salt out, meaning after extraction of basified liquid, seperate the solvent and wash it with an acidic solution (vinegar) to convert the alkaloid back into salt form therefore water soluble again. In essence it is a defat step aswell as oils will remain in the non polar region. After 3 x or more extractions of non polar solvent into vinegar can seperate it and evaporate the vinegar and be left with jim jam red goo. From there you have concentrated salt form alkaloids can refine further. Either do a dry tech converstion back to freebase and extract with acetone, or a variety of paths from there. You wont be left with cystals but can make changa or eliquid.

Thanks for your help; I really appreciate it. I'll look into those methods and hopefully get better results soon.

 

[_Trip_]

I did three pulls on the bark with just water and vinegar. The first pull was with 200ml of water, but I thought it was too little water, so I used 500ml for the second and third pulls.
What is salting out with xylene or dlimonene, how do I do that? Do I still freeze precipitate if I use those solvents?

Thanks!

Wait are you saying you didn't base it? What was you PH level when you did the pulls?

 

[dazultra]

Wait are you saying you didn't base it? What was you PH level when you did the pulls?

Sorry if I have my terminology wrong, I'm a noob.

- I cooked root bark powder water and vinegar for an hour (pH 4), strained it, then did that again another 2 times,

- then I added a saturated saline solution and NaOH solution to bring the pH to 14, I cooked that for an hour

- then I added the Shellite and cooked it for 20mins and then pulled the Shellite and put it through water to clean and repeated the last bit 3 more times and then let it evaporate and then froze.

Is the base part when you add the NaOH?

I have a pressure cooker and am thinking of using it for the initial bark cooking. I still have some Heptane; I guess I'll try that for the next batch along with the heat, but this time hotter.

 

[Bruce_Willis]

I tried doing this Tek a few times with heat baths, warming the solvent and shorter wait times but only got poor results, about 200mg.
Then I just did all room temperature and longer wait times and it turned out better. I'm not sure about the cooking of the bark business, I've never done that.

My exact notes from also doing this tek are as followed:

50g Acuminata root bark
500ml water
50ml vinegar
Added to 1L flask

(wait 24 hours)

60g salt dissolved in 200ml boiling water
60g caustic soda dissolved in 200ml cold water
Added to flask

(wait 24 hours)

100ml Shellite added to flask and gently mix several times over 1 hour.
Pull Shellite with pipette into glass containers and put immediately into the freezer.
(repeat above step 6 times)

Leave glass containers in the freezer for 24 hours then carefully decant solvent and dry crystals.

Pull1 = 150mg
Pull 2 = 93mg
Pull 3 = 95mg
Pull 4 = 95mg
Pull 5 = 100mg
Pull 6 = 0-2mg
Total = 533mg

Nothing amazing but happy to hit 1%. Good luck to you mate

 

[_Trip_]

Don't cook the base (the NaOH) or the naphtha the heat from the exothermic reaction with the NaOH is enough to heat the naptha if you do it at the same time for hot pulls.

Acuminata can be tricky sometimes. If you use heated shelitte it'll help but you'll want to shake it if you want the highest yeild if you get emulsion just add alittle more NaOH and shake again, repeat until the emulsion dissapears.
Doing this will result in higher yeild but form polymer dmt so it'll form a wax once you freeze precipiate and scrape it up.

Then use xylene on ya last pull too, this will help get the remaining dmt, do it separate to the naptha pulls (don't combine) and evaporate the xylene instead of freeze precipitate. It'll form an oil on evaporation, the oil is still majority dmt and can be used for changa it'll usually smells fruity too.

You could try evaporating some naphtha to increase concentration and freeze precipitate more dmt (but it shouldn't be necessary).

Waxy dmt is easy to work with and vape etc, no disadvantage over crystal dmt. Doing it like that will maximise yeild.

There are other ways salting dmt out etc using different solvents but that's the more straight forward way when working with acuminata. You should get approx 1.4-1.8% doing it that way.

 

[dazultra]

I tried doing this Tek a few times with heat baths, warming the solvent and shorter wait times but only got poor results, about 200mg.
Then I just did all room temperature and longer wait times and it turned out better. I'm not sure about the cooking of the bark business, I've never done that.

My exact notes from also doing this tek are as followed:

50g Acuminata root bark
500ml water
50ml vinegar
Added to 1L flask

(wait 24 hours)

60g salt dissolved in 200ml boiling water
60g caustic soda dissolved in 200ml cold water
Added to flask

(wait 24 hours)

100ml Shellite added to flask and gently mix several times over 1 hour.
Pull Shellite with pipette into glass containers and put immediately into the freezer.
(repeat above step 6 times)

Leave glass containers in the freezer for 24 hours then carefully decant solvent and dry crystals.

Pull1 = 150mg
Pull 2 = 93mg
Pull 3 = 95mg
Pull 4 = 95mg
Pull 5 = 100mg
Pull 6 = 0-2mg
Total = 533mg

Nothing amazing but happy to hit 1%. Good luck to you mate

Thanks so much for your detailed reply! Wow, that's interesting. I followed almost the same process as this on my first try and got 176mg and on the 2nd pull, I got tiny, almost nothing, but I didn't do the 1hour mix with the fuel. I think I did the first for a reasonable amount of time, but the next pull was quick, crazy to think there could have been loads more that I missed, I better be more patient next time. I would be pleased with anything close to 1% at this point; thanks again for the advice; I'll give it a go!

 

[dazultra]

Don't cook the base (the NaOH) or the naphtha the heat from the exothermic reaction with the NaOH is enough to heat the naptha if you do it at the same time for hot pulls.

Acuminata can be tricky sometimes. If you use heated shelitte it'll help but you'll want to shake it if you want the highest yeild if you get emulsion just add alittle more NaOH and shake again, repeat until the emulsion dissapears.
Doing this will result in higher yeild but form polymer dmt so it'll form a wax once you freeze precipiate and scrape it up.

Then use xylene on ya last pull too, this will help get the remaining dmt, do it separate to the naptha pulls (don't combine) and evaporate the xylene instead of freeze precipitate. It'll form an oil on evaporation, the oil is still majority dmt and can be used for changa it'll usually smells fruity too.

You could try evaporating some naphtha to increase concentration and freeze precipitate more dmt (but it shouldn't be necessary).

Waxy dmt is easy to work with and vape etc, no disadvantage over crystal dmt. Doing it like that will maximise yeild.

There are other ways salting dmt out etc using different solvents but that's the more straight forward way when working with acuminata. You should get approx 1.4-1.8% doing it that way.

Do you heat the naphtha separately and add it to a cooler base, I'm thinking over several pulls the base will cool?

Great idea with the xylene; I'll try that. Thanks! I would be over the moon if I could extract anything close to that.

Would waxy DMT be okay to use in a Vaporgenie Glass Sherlock? My other option is a vape cartridge.
Thanks heaps for the advice, I'm feeling more optimistic for my next try!

 

[acacian]

Waxy DMT should be fine.. acuminata extract is always a pretty smooth smoke in the GVG.

+1 on xylene. But I'd personally just pull with xylene to begin with and then clean it up with naptha afterwards if neccesary. Shellite/naptha requires heat and also you need to have it saturated enough to precipitate all of your DMT out.. If you pull with xylene first then you have all of your DMT in the one place and you can then dissolve in the minimum amount of shellite needed. Or you can salt your alkaloids directly out of your xylene with dilute acid and then re-extract via the addition of NaOH and fresh solvent.

Since shellite in Australia is such bad quality it always adds doubt in my mind with the initial pulls. It just doesn't seem very efficient. Xylene, toluene or DCM are much more trustworthy IMO.

 

[dazultra]

Waxy DMT should be fine.. acuminata extract is always a pretty smooth smoke in the GVG.

+1 on xylene. But I'd personally just pull with xylene to begin with and then clean it up with naptha afterwards if neccesary. Shellite/naptha requires heat and also you need to have it saturated enough to precipitate all of your DMT out.. If you pull with xylene first then you have all of your DMT in the one place and you can then dissolve in the minimum amount of shellite needed. Or you can salt your alkaloids directly out of your xylene with dilute acid and then re-extract via the addition of NaOH and fresh solvent.

Since shellite in Australia is such bad quality it always adds doubt in my mind with the initial pulls. It just doesn't seem very efficient. Xylene, toluene or DCM are much more trustworthy IMO.

So with xylene am I correct in thinking just add something like 100ml and shake for 20mins then pull and leave to evaporate. Then I can dissolve what I get in something like 50ml shellite or heptane with heat and freeze for 24hours then dry it out with a fan?
Are you also saying one pull will get all the dmt using xylene?
Thanks!

 

[acacian]

So with xylene am I correct in thinking just add something like 100ml and shake for 20mins then pull and leave to evaporate. Then I can dissolve what I get in something like 50ml shellite or heptane with heat and freeze for 24hours then dry it out with a fan?
Are you also saying one pull will get all the dmt using xylene?
Thanks!

Yes you can evaporate it or you can salt your alkaloids out with dilute acid and then make basic again before extracting with shellite.. me personally I’d just evaporate the xylene as it keeps other alkaloids in the mix that shellite might not - however salting out of your xylene means you can reuse it for future extractions. Narrow phyllode acuminata is mostly just DMT though so freeze precipitation with heptane would be the best course of action. Diggers shellite is a terrible solvent.

If you have heptane I wouldn’t bother using shellite.

For 50g plant material 100ml xylene will get everything out and doesn’t need to be heated.

 

[_Trip_]

Do you heat the naphtha separately and add it to a cooler base, I'm thinking over several pulls the base will cool?

Adding the lye will cause an exothermic reaction and heat the base anyway, just add the naptha afterwards or even before. The heat from the reaction is enough to heat the naphtha sufficiently. Just be cautious with heated solvents as per usual. You'll have enough time to do multiple pulls while it's warm.

 

[dazultra]

Yes you can evaporate it or you can salt your alkaloids out with dilute acid and then make basic again before extracting with shellite.. me personally I’d just evaporate the xylene as it keeps other alkaloids in the mix that shellite might not - however salting out of your xylene means you can reuse it for future extractions. Narrow phyllode acuminata is mostly just DMT though so freeze precipitation with heptane would be the best course of action. Diggers shellite is a terrible solvent.

If you have heptane I wouldn’t bother using shellite.

For 50g plant material 100ml xylene will get everything out and doesn’t need to be heated.

I've just got some xylene and am excited to try it this time. I've been cooking the bark in a high-pressure cooker, and the water has come out way darker, so I'm hoping this is a good sign! I'll keep doing it until the liquid fades in colour. Thanks for your advice; I'm going to try xylene and heptane.

Is narrow phyllode acuminate better than root bark? I can get either; I wasn't sure what the difference was.

Thanks again for the great advice!

 

[dazultra]

Adding the lye will cause an exothermic reaction and heat the base anyway, just add the naptha afterwards or even before. The heat from the reaction is enough to heat the naphtha sufficiently. Just be cautious with heated solvents as per usual. You'll have enough time to do multiple pulls while it's warm.

How long do you mix the naphtha with the base before pulling while it's warm? Is 20 minutes enough time and repeat it four times? Thanks!

 

[_Trip_]

Yh that's fine even 10mins with good shaking should be fine. Like I said if you get emulsion issues add alittle more lye at a time until it ceases to be an issue.