Almost no and 'fatty' residue

[froggydays]

Hi,

I tried my first pull and the results were not so good. I obtained only very little dmt which was quite 'wet' or fatty emulsion, which didn't really dry out after.

Steps:
100gr jurema root bark shredded
Moisturized, added half cup vinegar and 2 cups water
Boiled for 3 hours
Added some more water and vinegar during cooking to increase volume
Siphoned off the fluid into glass jar
Added NaOh 80gr/L to fluid until solution turned black
Added around 100ml naphta per pull
Pipetted naphta from top of solution after around 3 hours and froze overnight in glass lunch box with lid on.
Poured off naphta and let residue dry... around half a day.

Result: only the first pull showed something, however very little, just a small dot, and it was not dry powder at all. It seemed to remain wet from the naphta.

What am I doing wrong?

Thanks for any suggestions.

I hope to improve soon.

 

[TheGreenPhantom]

Sounds like a lot of naphtha. You might want to evaporate it for a few hours, then stick it back in the freezer.

 

[The Kraken]

Sounds like a lot of naphtha. You might want to evaporate it for a few hours, then stick it back in the freezer.

This ^^

Allow it to evaporate down by 40-60% then freeze precipitate.

 

[redbird]

In the future for pulling 100g, you can do 60ml for your first pull and 40ml for the subsequent pulls and have plenty of solvent to get it all in 4 or 5 pulls assuming good mixing.

Speaking of, you didn't describe your process there. If you just added the naps and let it sit on top for 3 hours before pipetting, that would be another factor contributing to low yields.
Hold one hand on top, one hand on bottom of your fimly closed vessel. Fully invert by pulling top hand towards that shoulder, then fully invert again pulling the originally bottom, now top, hand toward it's shoulder and repeat until you finish singing your ABC's.
Let settle a few minutes then repeat 4 more times before pulling off the solvent.

 

[froggydays]

In the future for pulling 100g, you can do 60ml for your first pull and 40ml for the subsequent pulls and have plenty of solvent to get it all in 4 or 5 pulls assuming good mixing.

Speaking of, you didn't describe your process there. If you just added the naps and let it sit on top for 3 hours before pipetting, that would be another factor contributing to low yields.
Hold one hand on top, one hand on bottom of your fimly closed vessel. Fully invert by pulling top hand towards that shoulder, then fully invert again pulling the originally bottom, now top, hand toward it's shoulder and repeat until you finish singing your ABC's.
Let settle a few minutes then repeat 4 more times before pulling off the solvent.

Thanks! I thought i wasn't supposed to mix the solution.

 

[froggydays]

This ^^

Allow it to evaporate down by 40-60% then freeze precipitate.

Thanks! I did try evaporating as the volume of naphta was quite high, although even with a fan after a few hours hardly any naphta evaporated. Any suggestions?

 

[Varallo]

Thanks! I did try evaporating as the volume of naphta was quite high, although even with a fan after a few hours hardly any naphta evaporated. Any suggestions?

This suggest you’re not using naphtha, which explains why you are having trouble.

Solution: backsalt in water with vinegar then base again and pull with proper naphtha and freeze precipitate.

 

[froggydays]

This suggest you’re not using naphtha, which explains why you are having trouble.

Solution: backsalt in water with vinegar then base again and pull with proper naphtha and freeze precipitate.

I'm not sure, I used Nafta that clearly says Nafta on the label. See attached. Which naphta do you recommend? Like zippo lighter fluid?

 

[Varallo]

I'm not sure, I used Nafta that clearly says Nafta on the label. See attached. Which naphta do you recommend? Like zippo lighter fluid?

I’m not familiar with this brand, so I can’t say for sure whether it’s suitable. It’s likely that it contains heavier or longer chains, which would make evaporation go slower. The solution, however, remains the same and is quite simple. If you used a large amount of naphtha instead of just a little, you can simply re-salt and go from there. Then add a base again and try the same process with a much smaller amount of naphtha.

 

[froggydays]

I’m not familiar with this brand, so I can’t say for sure whether it’s suitable. It’s likely that it contains heavier or longer chains, which would make evaporation go slower. The solution, however, remains the same and is quite simple. If you used a large amount of naphtha instead of just a little, you can simply re-salt and go from there. Then add a base again and try the same process with a much smaller amount of naphtha.

Thanks! Which naphta/solvent is preferred? Or what kind of naphta and where could I buy it? Like at a maintenance store is okay? or more like a paint/art shop?

 

[Varallo]

Thanks! Which naphta/solvent is preferred? Or what kind of naphta and where could I buy it? Like at a maintenance store is okay? or more like a paint/art shop?

FAQ - DMT Frequently Asked Questions and Troubleshooting Guide - DMT-Nexus Wiki

wiki.dmt-nexus.me

 

[froggydays]

In the future for pulling 100g, you can do 60ml for your first pull and 40ml for the subsequent pulls and have plenty of solvent to get it all in 4 or 5 pulls assuming good mixing.

Speaking of, you didn't describe your process there. If you just added the naps and let it sit on top for 3 hours before pipetting, that would be another factor contributing to low yields.
Hold one hand on top, one hand on bottom of your fimly closed vessel. Fully invert by pulling top hand towards that shoulder, then fully invert again pulling the originally bottom, now top, hand toward it's shoulder and repeat until you finish singing your ABC's.
Let settle a few minutes then repeat 4 more times before pulling off the solvent.

Thanks, but after inverting theres no need to let it sit for a few hours anymore?

 

[redbird]

Thanks, but after inverting theres no need to let it sit for a few hours anymore?

Right. The idea is you are mixing enough to create surface area for the molecule to migrate efficiently/effectively but not enough to cause emulsion. Then after you have done that 4 or 5 times you let it sit just long enough to get your clear separation layer again and then you pull.

 

[Icon]

Thanks! Which naphta/solvent is preferred? Or what kind of naphta and where could I buy it? Like at a maintenance store is okay? or more like a paint/art shop?

Naphtha is just a catch-all term for 'mixture of hydrocarbons'. You want light naphtha, which is a slightly more specific mixture of low-boiling hydrocarbons.

Review the wikipedia page for info.

Naphtha - Wikipedia

en.wikipedia.org

Look up the MSDS for brands you're considering, it should describe the ratios of hydrocarbons or the boiling point range.

But as Varallo said, you can use what you have, as well as many other things, if you take the time to learn the mechanics involved.

 

[froggydays]

Naphtha is just a catch-all term for 'mixture of hydrocarbons'. You want light naphtha, which is a slightly more specific mixture of low-boiling hydrocarbons.

Review the wikipedia page for info.

Naphtha - Wikipedia

en.wikipedia.org

Look up the MSDS for brands you're considering, it should describe the ratios of hydrocarbons or the boiling point range.

But as Varallo said, you can use what you have, as well as many other things, if you take the time to learn the mechanics involved.

Thanks! I read in the description of this nafta that the boiling point is more than 200 degrees Celsius, so very heavy. Maybe this is one reason. (Wiki: Heavy naphtha boils between 90 and 200 °C)

 

[Icon]

Thanks! I read in the description of this nafta that the boiling point is more than 200 degrees Celsius, so very heavy. Maybe this is one reason. (Wiki: Heavy naphtha boils between 90 and 200 °C)

Correct. The evaporation rate will be low in that case, making that method time consuming. And the solubility will be too high to freeze precipitate.

But there should be DMT in there. What you want to do is back-salt.

Warm up a half cup of vinegar, then add 1/3 of it to the dmt-nafta, mix well. DMT will move back to the vinegar. Separate the dmt-vinegar and repeat the wash 2x with the rest of the warm vinegar.

Then re-do what you did before, starting from the NaOH step, except swap in a different solvent at the end. Could be light naphtha; or heptane, hexane, pentane, etc.

 

[froggydays]

Correct. The evaporation rate will be low in that case, making that method time consuming. And the solubility will be too high to freeze precipitate.

But there should be DMT in there. What you want to do is back-salt.

Warm up a half cup of vinegar, then add 1/3 of it to the dmt-nafta, mix well. DMT will move back to the vinegar. Separate the dmt-vinegar and repeat the wash 2x with the rest of the warm vinegar.

Then re-do what you did before, starting from the NaOH step, except swap in a different solvent at the end. Could be light naphtha; or heptane, hexane, pentane, etc.

Thanks, I'll try it when I receive the lighter naphta

 

[froggydays]

Went much better this time I think! I used regular Zippo lighter fluid this time.

I had some problems with the inverting as I did not have a good cork or pot to invert in; as the boiled MHRB was still quite hot especially after adding the NaOh, the lid of the pot I had popped off a few times... However, the rest went well.

As @redbird mentioned I did not after inverting let the naphta sit for a few hours as I did before, but just waited for it to settle at the top and then pipetted it off for freeze precipitation.

The result of the first pull is in the picture, a lot more than in my first try. I do notice there are some yellow slabs but the rest is mostly white. Should it be all yellowish?

The second pull did not contain so much, about 1/8th of the first one I think.

 

[froggydays]

Thanks, I'll try it when I receive the lighter naphta

I tried it now freezing. However, I maybe didn't add enough NaOH to the volume. I took the standard 80gr/L but in this case the solution is pure vinegar.

I ended up with around 200ml of solution (ie vinegar) and added only 20gr NaOH. I think in retrospect unfortunately this probably hasn't increased the pH high enough.

 

[Transform]

I tried it now freezing. However, I maybe didn't add enough NaOH to the volume. I took the standard 80gr/L but in this case the solution is pure vinegar.

I ended up with around 200ml of solution (ie vinegar) and added only 20gr NaOH. I think in retrospect unfortunately this probably hasn't increased the pH high enough.

Yes, the 10g of acetic acid (assuming a vinegar at standard 5% w/v) would require (10/60)*40g = about 7g NaOH to neutralise. The remaining 13g likely won't have been enough to react with all the bark tannins, etc.