Toluene STB

[AlchemicalGnostic]

So I'm starting an extraction today using toluene as the NPS. I plan on doing 150g of mhrb with 75ml of toluene for each pull. I plan on doing 4 to 5 pulls and combining them all and evaporating. On the evaporated product I'm gonna pull with naphtha to pull all the spice into the naptha.

What am I left with? I remember reading a report by burnt that jungle spice is mostly nn dmt.
If i pulled all the dmt out of the tolune evapped product, fats and oils are what's gonna be left behind right? Or will there be small amounts of other trace alkaloids left behind?

Here's the jungle spice analysis by burnt:

Summary of jungle spice analytical work - Plant Analysis and Substance Testing - Welcome to the DMT-Nexus

 

[melotikaci]

I prefer doing 7-8 pulls with naphtha, it will get most of the dmt out, and then 2-3 pulls with toluene for jungle spice. I think that's better way for "managing" spices

 

[AlchemicalGnostic]

I was going to pull with toluene initially and evap it and then do one or two naphtha pulls to get all the spice out of the 'jungle spice' product.

This way I eliminate most of the naphtha pulls.

My question is, if 'jungle spice ' is mostly dmt, then what will I be left over with after I pull with naphtha? NMT? Yuremamine? plants and oils?

 

[Jees]

Good luck with evaporating toluene from a sticky oily substance. It's going to smell toluene forever and forget about 'dry'. I estimate that residual toluene will carry the oily characteristic into your naphtha pulls making those also oily.

The human solution to this is to backwash the toluene with an acidic water, and re use the toluene later.

 

[AlchemicalGnostic]

Good luck with evaporating toluene from a sticky oily substance. It's going to smell toluene forever and forget about 'dry'. I estimate that residual toluene will carry the oily characteristic into your naphtha pulls making those also oily.

The human solution to this is to backwash the toluene with an acidic water, and re use the toluene later.

Are you talking about salting out the spice with a FASW?

In the jungle spice analysis I linked burnt described the method I have described above.

SWIM thinks its best to go from a stronger less selective solvent like toluene or d limo and then use hexane or naptha to clean up that jungle spice residue.

Couldn't i just re x the jungle spice product til I'm satisfied?

 

[downwardsfromzero]

Doesn't need to be FASW, vinegar or just about any other sufficiently acidic liquid will do.

Couldn't i just re x the jungle spice product til I'm satisfied?

^it's suggested that this might be difficult:

that residual toluene will carry the oily characteristic into your naphtha pulls making those also oily

Perhaps a good defat during an initial acidification might be in order, if you only have toluene to play with. (You'd need naphtha or heptane for a recrystallisation, ideally.)

 

[AlchemicalGnostic]

So is burnt's suggestion to use a stronger solvent like toluene and cleaning it up with naphtha outdated or is it just too difficult and messy?

To salt out with vinegar, I simply slowly drop vinegar into the toluene. Separate the vinegar and evap to get dmt acetate? Then I use sodium carb to convert to free base? Am I understanding this right?

I've been hesitant about salting but I gotta try it at some point!

 

[AlchemicalGnostic]

okay I decided to go ahead and do the toluene pulls and salt out with vinegar.

If I do 5 75ml toluene pulls and combine them to have 375ml. I would do 3 vinegar pulls of 75ml each on the toluene and evaporate it to retreive the dmt acetate. Then I'd add 1/1 ratio of dmt acetate to sodium carb and a tad bit of water say 5ml? Then do 3 ethanol pulls on powdered product to get dmt fb.

I think I have this understood correctly.

 

[Jees]

You only need one acid pull on the toluene, if the pH after the pull is still 3 to max 5 you are set. You can do a second one for peace of mind but not really necessary I think.

Evaporating such acid water is preferred over evaporating pure toluene.
Your acid water will smell like toluene but now it is traces of toluene only.
Evap volume down til oily, add new plain water + mix, evap down, add maybe some ethanol if you have, evap down, ..., till there is no more toluene smell.

If muriatic acid is used then also the excess acid will evaporate in the process and in the end pH will normalize after a few evaps to 5 or so, thus safe.

This process is used on chaliponga leaves with good result, and yes it stays a bit sticky and will hold some none active components but you do have full spectrum actives.

Then you can indeed base with sodcarb and pull with ethanol as you say. Expect no dry result, chances are you will get something sticky but potent. It will be full spectrum!
If you pulled with naphtha instead of ethanol you get the nn-dmt, but be careful with heat as very warm naphtha does take dmt oxide in it!
Then pulling with ethanol for the rest, prolly dmt oxide, just as potent.

Fresh wood will be a less oily result than old wood. I've seen wood with near none dmt oxide, and old wood with 50% nn-dmt and 50 % dmt oxide (long time open air stored somewhere?). It was reduce-able with zinc so really pointing to dmt oxide.

...So is burnt's suggestion to use a stronger solvent like toluene and cleaning it up with naphtha outdated or is it just too difficult and messy?

Now if you have 1.6 to 2% readily with naphtha pulls alone on the wood, I recon there's no use to hunt for the oxides and consider toluene pulls as unnecessary. But if your naphtha pulls on the wood give like 1% yield, chances are you have old wood with just as much dmt oxide waiting to be ignored or pulled with toluene.

1- the mini ab step is incorporating a cleaning up step;
2- the toluene pulls very powerful on the wood and needs no warmth at all, room temp is OK.

All is said relating to mimosa H.

 

[Jees]

...You only need one acid pull on the toluene, if the pH after the pull is still 3 to max 5 you are set. You can do a second one for peace of mind but not really necessary I think.

Evaporating such acid water is preferred over evaporating pure toluene.
Your acid water will smell like toluene but now it is traces of toluene only.
Evap volume down til oily, add new plain water + mix, evap down, add maybe some ethanol if you have, evap down, ..., till there is no more toluene smell.

If muriatic acid is used then also the excess acid will evaporate in the process and in the end pH will normalize after a few evaps to 5 or so, thus safe.

This process is used on chaliponga leaves with good result, and yes it stays a bit sticky and will hold some none active components but you do have full spectrum actives....

This is such chali extract result as mentioned, 3.2% yield clearly with a lot of plant matter but leaving it just like that. There are visibly crystals in the 'semi hard honey'. No way of re-X that, one would need naphtha for that so loosing all the precious (near) full spectrum components.
If anyone has deviating or adding thoughts (preferably based on experience) please do. E.g. a clean up without losing full spectrum potency.

 

[AlchemicalGnostic]

Thanks! This helps a lot!

So after basing with sodium carb, I can pull with naphtha and freeze precip instead of ethanol and evapping?

The ethanol will give a full spectrum product, while the naphtha will select the nn dmt?

I was originally gonna try pulling with toluene and evap then clean up with naphtha but it seems its not that recommended as one thought. So now I'm gonna deplete the bark with naphtha like I normally do then do the toluene pulls and attempt my first ever salting step!

Nice crystals! Those were from a toluene pull?

 

[Jees]

So after basing with sodium carb, I can pull with naphtha and freeze precip instead of ethanol and evapping?

I suppose so. I've not used sodium carb so far before making a pull with whatever.

The ethanol will give a full spectrum product, while the naphtha will select the nn dmt?

Yes, but be aware that ethanol is going to drag a lot of plant matter too.
Naphtha is selective to nn-dmt if not too warm. The hotter it gets the more it potentially does take the dmt oxide, leading to more oily results. Not only dmt oxide but also plant matter. Luke warm is okay to be selective on NN.

Nice crystals! Those were from a toluene pull?

Yes toluene, backwashed, evaped the backwash several times for the residual toluene and acid to disappear. I told that I believe?
Not so nice crystals I think, a bit of a mess but doing the job wonderfully for oral purposes.

Very comparable result picture to what jamie did here:
iso tek for chaliponga/leaf sources.

I could consider to re-vinegar my material, dump sodcarb on it, and re-pull with iso or ethanol, as an extra step. All in all jamie did quite well skipping any toluene or xylene pulls.

 

[syberdelic]

If you want to use a stronger solvent for the non-polar stage, I would highly recommend xylene over toluene. It smells awful and will take a long time to evaporate, but you shouldn't have any problem getting it to fully evaporate even out of oily substances.

 

[Jees]

If you want to use a stronger solvent for the non-polar stage, I would highly recommend xylene over toluene. It smells awful and will take a long time to evaporate, but you shouldn't have any problem getting it to fully evaporate even out of oily substances.

I wonder about that. Toluenes vapor pressure is 3 times that of xylene indicating more volatile, backed up by its boiling point 30 deg C lower than xylene. Did I miss out on something here?

 

[syberdelic]

If you want to use a stronger solvent for the non-polar stage, I would highly recommend xylene over toluene. It smells awful and will take a long time to evaporate, but you shouldn't have any problem getting it to fully evaporate even out of oily substances.

I wonder about that. Toluenes vapor pressure is 3 times that of xylene indicating more volatile, backed up by its boiling point 30 deg C lower than xylene. Did I miss out on something here?

I could be wrong here but; From back in my painting days; toluene is used as a thinner and base for oil based paints specifically because it never (or at least many years) completely dries out when combined with the pigments and other components of paint. When oil based paints do completely dry, it gets so dry that it cracks and crumbles off the painted surface. I know there is some truth to this because when I tried using toluene to clean my brushes, hours later they would still be oily and I would have to wash them again with acetone or paint thinner.

Again, I could be wrong about the details but this is the advice I received and my experience.

 

[Jees]

Ah paint yes. I don't know much about that.
I think we can rely on the lab numbers though, I checked MSDS of T and X.
Internet is awesome

 

[Mindlusion]

I think its actual oil in the oil-based paints that keeps it from drying, when the linseed oil finally evaporates, that is when you get the dried out paint. Toluene just thins.

Toluene and xylene will definitely leave some traces on evaporation, not to mention industrial grade solvents may have some high boiling impurities.

Toluene comes off faster than xylene, but removing both of them from residues can be tough, even under high vacuum pump solvent, it takes a lot of time, traces are detectable for quite a while. So maybe some truth to the painting, probably why it is such a great thinner.

Toluene and xylene are both excellent solvents for dmt extraction, they are my preferred. Naphtha has too many limitations, wasteful and is time consuming. But you should use FASI/FASA to salt out the fumarates, that way xylene can be poured off and the traces are easily removed.

 

[pitubo]

I think its actual oil in the oil-based paints that keeps it from drying, when the linseed oil finally evaporates, that is when you get the dried out paint. Toluene just thins.

Actually, classical oil paint does not dry by evaporation, it dries by polymerization.

 

[downwardsfromzero]

I poured some sulfuric acid on some linseed oil in a sink once. Instant polymerisation made the clean up process rather difficult.