Something went wrong - Max Ion Tek

[ChemicalEnthusiast]

So something went wrong with this last extraction I did.

I used the exact same bark that I've used previously but I used a different tek.

I performed the max ion tek with 500g with a few differences from the main tek:

1. Warm acidic bath with just enough acidic solution to cover the bark for 8 hours, stirring occasionally
2. Added 1 L salt solution
3. Based solution then warmed the solution for ~2 hours stirring occasionally
4. Pulled 5 times with 250 ml warm naphtha
5. Lastly a mini A/B then freeze precip

I reduced the volume of the pulls down to 500ml (1ml/1g bark) and this is where I started to think something went wrong, the solution didn't get cloudy at all. I still freeze precipitated the solution and I was left with very little DMT (probably .5g or less, its still drying as I type).

I can only think of a few places where things went wrong.

On the initial pulls I decided to not let the based solution cool down. Is it a necessity for the based solution to cool down before pulling? If so, why?

The only other place where I could see something going wrong is that I did not pre-evap enough. Is pre-evaporating to a certain volume a necessity? My initial guess was no but now I'm thinking I should have pre-evaped more.

Any advice and comments are greatly appreciated. I really want to figure out what went wrong so it doesn't happen again.

I've 4 successful extractions with 100g yielding ~1.5 g white crystals each time and its very discouraging to perform a larger extraction and not get anything :/

 

[ChemicalEnthusiast]

After searching the forum I think (hope) the problem is that I didn't pre-evap enough. I am currently evaporating down the solution to a much smaller volume. I'll probably go down to ~200 ml or even less. Fingers crossed!

 

[ChemicalEnthusiast]

So I reduced the volume of the pulls and I ended up yielding just over 1 gram but I should have yielded much much more considering how much bark I used.

I really would like to know where I went wrong :/

I don't think the max ion tek is the best tek for larger amounts of bark.

I will be attempting a 500g extraction using my old tek very soon and hopefully that will be more successful. It will require more steps and more equipment but I am much more confident with that tek so I expect good results.

 

[DreaMTripper]

If you didnt let it cool you may have pulled some oils that interfere with the precipitation, try evaporating down to 75-100ml it could be still in there. My hunch is at 200ml it isnt saturated enough to precipitate all of it anyway. If no luck evaporate it all away or do a mini-acid base.

 

[cyb]

I really would like to know where I went wrong :/

You used too much solvent to pull with.
You didn't evap down enough before freezing.
Maybe you messed up the mini A/B

Your bark maybe low in alks.
You may have overdone the ingredient amounts.
Also, you deviated from the tek.

Could be so many things.

I don't think the max ion tek is the best tek for larger amounts of bark.

Please don't blame the technique if you change it up and don't fully understand what you're doing

 

[ChemicalEnthusiast]

Please don't blame the technique if you change it up and don't fully understand what you're doing

I apologize for the way that came off. I think that your max ion tek is the most sophisticated tek around. I just found it very difficult to work with that amount of bark.

Your bark maybe low in alks.

I used the exact same bark (leftover from previous extractions) so I don't think this was the issue.

You used too much solvent to pull with.

Is it possible to use too much solvent? Wouldn't more solvent allow for more contact with the aqueous solution?

Also, you deviated from the tek.

The only place that I deviated from the tek is not allowing the base solution to cool down. Is this really an issue? Many other teks emphasize to NOT let the solution cool down and that is why I chose not to.


After thinking for quite awhile on this I think I have a good idea about what went wrong. I used powdered ACRB and this made the solution basically mud. Due to the consistency of the solution I think that it was hard for the solvent to penetrate into the mud and extract all the alks. Does this make sense?