New A/B extraction....yield problems.

[OrangeShade]

Greetings all. SWIM has performed 3 different extraction methods so far with varying results. The last extraction SWIM performed was a STB using Spicey Cat's tek

(Hip Forums)

This produced a good yield using 100g MHRB. The ratio for this extraction was 100g MHRB - 850ml water - 125g NaOH. After the freeze precip process, a large amount of crystals formed in the jar that resulted in a very slightly off white powder as an end product. SWIM would say it was nearly a gram. A fairly clean smoke, short but intense/clean visuals.
Always looking to experiment and improve, SWIM decided to try an A/B extraction (first time)and this is where SWIM thinks he has gone wrong.

This A/B tek suggested 25g NaOH-1 litre de-ionised water-100g MHRB. SWIM doubled up the experiment using two seperate jars containing 100g of bark in each and combining then evaporating approx 50 percent for the freeze precip process. At present SWIM is at the final extraction of the product from the non-polar solvent from the freezer. Although the crystals look very white and sparkly, SWIM can see that there is definately not 2g or even close to of crystal.

My main questions are:

1. Has using much less NaOH for the A/B tek contributed to a much more reduced yield?

2. SWIM still has the two jars containing the bark/NaOH solution, perhaps there is more still in there?

3. Should SWIM just revert back to the tek that I know works and is there any point doing a A/B tek when the STB is easier and seemed to produce a better yield.

4. Also, Just your thoughts on this one, SWIM keeps reading about fellow travellers breaking through on 60mg of freebase, where it has taken nearly 100mg of freebase to do the same for SWIM. For example, can you have 100mg of dmt that is equal in potency to 60mg of purer product? Perhaps SWIM was losing product during the smoking process, overheating/underheating? SWIM is pretty well versed with psychedelics, consumed a fair bit of acid over the years. But that should not have any effect on the tolerance of dmt, surely?

I look forward to your comments.
Peace :d

 

[d*l*b]

Hi OrangeShade–

I am a little confused by your description quoted below – do you have any information on the acid stage?

This A/B tek suggested 25g NaOH-1 litre de-ionised water-100g MHRB. SWIM doubled up the experiment using two seperate jars containing 100g of bark in each and combining then evaporating approx 50 percent for the freeze precip process. At present SWIM is at the final extraction of the product from the non-polar solvent from the freezer. Although the crystals look very white and sparkly, SWIM can see that there is definately not 2g or even close to of crystal.

1. Has using much less NaOH for the A/B tek contributed to a much more reduced yield?

Without knowing the pH achieved that would be a difficult question to answer, did the solution turn black on adding the NaOH?

2. SWIM still has the two jars containing the bark/NaOH solution, perhaps there is more still in there?

Quite possibly, how many pulls have you done and how much solvent have you used? I generally stop pulling at 5 or 6 pulls, but I have seen (albeit small amounts of) product being pulled on the 9th pull. Amount of pulls to get everything will be dependent on amount of basic solution being pulled from, amount of solvent, type of solvent and temperature.

3. Should SWIM just revert back to the tek that I know works and is there any point doing a A/B tek when the STB is easier and seemed to produce a better yield.

I am heavily biased in favour of A/B, it produces equal yield, is cleaner, can be filtered and reduced in the acid stage and doesn’t require you to work with such massive amounts of basic solution.

4. Also, Just your thoughts on this one, SWIM keeps reading about fellow travellers breaking through on 60mg of freebase, where it has taken nearly 100mg of freebase to do the same for SWIM. For example, can you have 100mg of dmt that is equal in potency to 60mg of purer product? Perhaps SWIM was losing product during the smoking process, overheating/underheating? SWIM is pretty well versed with psychedelics, consumed a fair bit of acid over the years. But that should not have any effect on the tolerance of dmt, surely?

Some people need to dose more than others, but in my experience most of the issues are actually in smoking tools and technique, set and setting.

 

[OrangeShade]

Thanks for the reply. Sorry for the sparse info, this is SWIM's third extraction of this wonderful sacrement and is hoping to learn and perfect a single extraction method that he can do every time to produce some quality spice. Basically the tek SWIM followed went like this:

NB: No litmus papers used

1. Added 1 litre of de-ionised water (battery top up water) to a screw cap bottle, added 25g of NaOH.
2. Once cooled, added 100g MHRB, shaken for a few minutes and left overnight (speeded up process in a warm water bath was an option). Solution went black as in previous extractions (all two of them )
3. Warmed up Naptha (Ronsol lighter fluid) in a hot water bath and added to the mix (3 x pulls of 40ml naptha). Gently tilting/rolling the naptha in the mix for 10 minutes and letting settle for 15mins each time. Confirmed visualy that the amount of naptha had settled to the top again was equal to what was started with. Pulled this into a jar, then decanted a second time to remove any impurities and put in a pyrex dish.
4. Once all the naptha was now in the pyrex dish, evaporated approx half of this.
5. Just before half of this evaporated, the naptha went very cloudy and large deposits of white were seen to crash out of the solution. The solution then went a little bit clearer.
6. When the naptha was placed in a jar for the freeze precip process the left over "white substance" in the pyrex dish dried almost instantly. It was whiter than SWIM's previous extraction a few weeks ago end product after re-crystalising! And it had sparkly crystals in it.

After 3 days of the spice being in the freezer (SWIM rotated 12hrs in freezer then 4 in the fridge, back in for 12 in the freezer etc..) SWIM produced 1.1g of fairly white crystal structure. Had a lot more structure than previous attempts (looked a lot more like crystal as opposed to powdery spice he pulled before). The powder scraped up from the pyrex dish after evap'ing and before the freeze precip process amounted to approx 200mg. Working it out 1.3g of spice from 200g MHRB gives 0.65% yield? How does this sound to other psychonauts?

SWIM thinks, to be fair to this above tek, it has produced some really nice crystals, better than the STB tek he used before. Just seems a smaller yield. An easier process and much less NaOH compared to spicey cat's tek (125g NaOH-850ml H2O-100g MHRB). The only real difference it seems was using de-onised H20 (battery top up water) as opposed to normal bottled H20.

From this point, SWIM is thinking is it also worth re-x with this pretty good looking already crystal to further purify? SWIM has 300g of root bark left and is deciding which tek to follow for the remainder.

Hope SWIM has covered everything! Thanks again.

 

[OrangeShade]

Here's a pic. The pile on the left is 1.1g (no re-x performed yet). Pile on the right is .2g of the stuff scraped from the dish before the freeze precip process.

http://i183.photobucket.com/albums/x4/leeshaw78/Extraction3prex.jpg

 

[Noman]

That's not an A/B.

 

[OrangeShade]

That's not an A/B.

Ah there lies the problem then. What tek has SWIM done then? Seemed to produce a pretty good spice in terms of crystal formation/whiteness as in the photo. Yet to try how it smokes though.

Currently SWIM is doing another 2 pulls from each jar containing 100g MHRB in each, to see if he can obtain any more spice. These jars have been sitting there for a couple of days in the NaOH/de-ionised water solution.

Any thoughts on if this works and SWIM can obtain the remainder 30-35% from the other jars whether or not this is an ok procedure to follow? Is SWIM doing anything majorly wrong that will affect purity?

 

[OrangeShade]

Just an update on this thread. SWIM smoked the crystal spice obtained and broke through on approx 60mg. Very clean, intense visuals. Something worked!
SWIM wonders what the point is doing all these other tek's when a simple and straight forward one does the job. SWIM will definately be repeating this. Just need to try and increase the yield somehow. Any ideas on how to do this, is SWIM missing something perhaps, more pulls, less naptha perhaps? Your thoughts are appreciated.

 

[d*l*b]

That's not an A/B.

Ah there lies the problem then. What tek has SWIM done then?

The tek you did was an STB (Straight To Base) as opposed to A/B (Acid/Base).

A/B is useful for working with oily material (you can remove fats in the acid stage), you can filter the solution (solvent and basic MHRB soup separate almost straight away and you can use a separatory funnel if you want), and you can reduce the solution (for instance I would typically boil it down to 200ml before adding NaOH). For me, despite the extra steps working with A/B is worth it.

SWIM wonders what the point is doing all these other tek's when a simple and straight forward one does the job.

Different strokes for different folks I guess. For me for instance I would find the tek you use a bit too gloopy, I used 1.6L water per 100g bark. Now I do A/B rather than STB for the reasons I described before.

Any ideas on how to do this, is SWIM missing something perhaps, more pulls, less naptha perhaps?

MHRB I have seen so far has contained 0.7–1.7% DMT so even if your bark isn’t great there should still be spice to be had there. Try doing more pulls until nothing more can be retrieved. You can also warm your solution to make the naphtha pull up more.

 

[OrangeShade]

Ah Ok so maybe A/B is the way to go then. SWIM will try for the next batch. From what it looks like so far, SWIM will obtain about 3.5g of spice from 500 bark. Probably not that good in terms of yield. SWIM still has 2 jars each containing 100g bark solution in each. Will try as you said, heat solution and pull some more hopefully. Should SWIM increase the water content of the jars to pull more. ie. add more de-ionised water to bring it up to 1.5L of water? Will this make it any easier to pull more or just leave as is and pull from the slightly heated solution?