My first extractions.

[OrangeEnergy]

Firstly, I would just like to give a massive bigupyourself to everyone on here spreading the knowledge and love.
I started my first extraction on the 15th, and have just done the first pull of this using Clipper lighter fluid for nps.
In the run-up to this, I've been reading lots, and used cybs hybrid tec for the first extraction, and MaxIon tec for the second extraction, the freebase of which is currently cooling down, and I have sourced some 99.5% Heptane for this (and further purifications).

The first extraction was something of a drawn out affair, due to putting together equipment etc.
Here are the timings, as, as you will see, I am very surprised at how much I got from the first pull using 50ml Clipper. I have only done two pulls so far, and crystallised both separately to compare.

15th 2pm : 50g bark 200ml dist H2O +60ml vinegar.
Cycle heat/cool and stir until 7pm.
16th 8am heat +stir. 4.30pm filter. add nacl soln. add NaOH. 5.30pm warm freebase. Allow to cool and add 50ml nps.
22nd 5.30pm pull solvent and put in freezer. 6.30pm add 40ml solvent (all I had). Mix x4. Pull and put in freezer.
23rd 8am pour off solvent and dry under fans.

First pull has provided 0.20g spice Second pull very little, and the ramekins will not be being used again as dreadful for getting product out of! Glassware on order.


Am going to pull first freebase mix again, using recovered clipper lighter fluid, to see what else may be left in there, as there should be lots.
Keeping this solvent seperate so all future pulls will be pure heptane.
Will keep updating...

 

[downwardsfromzero]

Nice to see some good results, 0.4% seems fair to middling, although I suspect that's down to your bark. You might want to try doing your naphtha pulls on the soup while it's still warm - this will save you time and should also improve the yield.

I'd be incline to say the heptane might be best save for doing recrystallisations but it will serve perfectly well for pulls if the mixture is kept warm (water bath - no ignition sources!) It's not exactly cheap so you may want to take steps to minimise its evaporation and maximise the amount you get to re-use.


Ramekins do look convenient but, as you have found out, they are fiddly if it's anything but the very low-sided ones like you get for certain brands of crème brulée. One possible solution - no pun intended - is to wash the material out with something like acetone and allow it to evaporate in a more accessible vessel. It will be gooey at first (acetone is hygroscopic) but it should firm up into a quasi-crystalline mass eventually.

 

[OrangeEnergy]

Nice to see some good results, 0.4% seems fair to middling, although I suspect that's down to your bark. You might want to try doing your naphtha pulls on the soup while it's still warm - this will save you time and should also improve the yield.

Cheers. Just to clarify, that was from two pulls using 50ml+40ml lighter fluid . Solvent had been left in alkali far too long (couple of days), so spice will certainly not be the purest, but am still waiting for equipment to arrive (postie literally just arrived. Almost there, just need pipette!).
Quite pleased with the pull, and reckon once I'm all geared up for multiple pulls in a session, my yield should be pretty good.
Now have stuff for infusing IPA to make some changa blends

 

[OrangeEnergy]

One possible solution - no pun intended - is to wash the material out with something like acetone and allow it to evaporate in a more accessible vessel. It will be gooey at first (acetone is hygroscopic) but it should firm up into a quasi-crystalline mass eventually.

Is there a reason people don't seem to use heptane when it is easy to get delivered? The pull I did with it compared to lighter fluid naptha was so much nicer. Is it just a price thing?

 

[downwardsfromzero]

It's mostly a price thing when it comes to evaporation, although I suggested acetone because DMT is way more soluble in that than it is in room temperature heptane. This means you have a much smaller amount of solvent to evaporate afterwards - and acetone evaporates more quickly* than heptane.

The selectivity you see with heptane could also be considered to be advantageous, and you could use it warm to clean out your fiddly precipitation ramekin and then repeat the freeze precipitation with a more concentrated solution in a more convenient vessel - seeing as you already have the heptane.

One final thing is that my preferences are moulded by what can be obtained off-the-shelf rather than via online ordering. This is something that varies between locations, but I can get cans of acetone much more easily than I can get heptane. (In case you were wondering )

*Although acetone is a bit hygroscopic so there may be a slow-to-evaporate watery reside at the end.

 

[OrangeEnergy]

Nice. I figured that must be it. I'm happy to pay a bit more for the solvent, as it's just so much nicer to work with! First enhanced leaf a success

 

[OrangeEnergy]

Time for update on progress.
So, I'd done two 50g bark extractions, first using naptha and the second heptane. Good learning processes with reasonable results and my first attempt at enhanced leaf was a success!
This week I have taken the rest of my bark (890g), warmed it in some acid, freeze and thawed the mix twice, and then acid cooked the mix with low heat on and off for a couple of days, temp never getting above around 45C.
I then strained through muslin and again through coffee filters and now have all that acid solution in a big demi-john in my cupboard. I thought I'd do this first step in bulk, and then extract from that soup as I need.
I have taken 260ml of this soup, added salt and then basified and pulled with 4x50ml of heptane. This has been in the freezer a day and a half, and I am very happy with the results. Lots of white crystals!
Now to make some vape juice
Crystals under the fan. Will weigh and post result in a bit.

 

[OrangeEnergy]

0.53g