A/B vs STB Comparison (pics) + FINAL TALLY!

[jbark]

Wow! Who would have guessed, with all I have posted, that THIS would be my most popular AND most contentious post!! Trickster, i am glad you have brought this to our attention. I think the best course of action would be to correct it in the wiki, where it is listed as an A/B. Not being a chemist and having no interest in getting into the nitty-gritty of defining what exactly constitutes an A/B extraction, I must defer, for now, to the wiki, my (and most's) only reference. If you succeed in getting Panoramix's tek moved to the STB section, I will more than gladly change the name to something more appropriate. In the meantime, I shall consider it an A/B.

Cheers,

JBArk

 

[jbark]

I use an A/B technique with powdered MHRB, and have discovered that there are several misconceptions perpetuated by most TEKs. I haven’t posted these before, because I’m not interested in arguing or defending these points. These are observations I’ve made after much experimentation:

1 ----- Very little if any acid has to be added to the bark powder. I’ve never tried using no acid at all, but as little as 50mL of 5% acetic acid in 2L of water yields the same results as much more. My guess is that most/all of the DMT in MHRB is already in salt form. I bet that acid has little to no effect on yield.

2 ----- Boiling of the acidified solution is totally unnecessary. Some TEKs call for soaking/boiling for hours. I add hot (not boiling) water to the MHRB powder, stir it a few times, then let it settle. I then siphon off the liquid and repeat 3 more times.

3 ----- Filtration is unnecessary. Many TEKs use messy and wasteful filtration procedures to separate the liquid from the MHRB. This is not necessary. Allowing the solution to settle for 30-45 minutes and then siphoning off the clear liquid is a much cleaner and less wasteful way to do separations.

4 ----- Gentle boiling or slow simmering for reduction is not necessary. I do my reductions at a full boil. There is no loss of product that results from vigorous boiling, and over 1L of liquid can be reduced to 200mL in about 15 minutes. Depending on your stove, you might even reduce it faster than that.

5 ----- No separatory funnel is needed. Once the DMT-containing liquid is reduced, it can be processed in the same manner as a STB – the solution in a jar/bottle is basified (using far less base than STB), non-polar solvent is added, and the extraction proceeds like STB. No need for expensive equipment.

These adjustments make for a very quick and easy A/B with very good yields. (I’ve had yields of 1.75% with MHRB from a vendor known for high quality MHRB.)

Thanks for this Gibran2, thorough as usual! - although I quite expect your parameters would also perhaps disqualify it as an A/B if a new definition were arrived at.

I suspected most of those techniques were superfluous, which is why I chose 2 teks that avoided them. I will post yield results and an evaluation soon.

JBArk

 

[jbark]

It looks like theres a bit of an emulsion on the jars. Crazy shaker you. And I cant really see you at all, maybe get a better accidental picture.

The Naptha looks nice, So do the crystals, Essacly what SWIMs looked like when he used my freezer one time. The yellow isnt fats I dont think (since MHRB is extremely anorexic ~.o not much fat at all), its probably oil/oxide mixture, I get that a lot.

have you noticed any changes in the color of the naptha leaving them in for longer times? Did you use heated naptha?? I find that using heated increases yeild (just a bit) but brings a bunch of contam with it.. weird....

Lewkin gewd so faaaaar!

-gir

Gir - I think the emulsion you refer to is in the A/B batch, and it is just MHRB crusty bubbles - unless you mean the closeup of the STB jars, in which case I took that goop to be plant lipids and general guck. The naptha seperated nicely and sat atop the gunk.

No, no colour difference, although maybe... the first pull was a little yellowish, while the others were all colourless. And yes, all the naptha was heated, as per your tek!

JBArk

 

[jbark]

First off, Panoramix's is not exactly an A/B, but rather an STB with an acid pre-soak. So it is hardly a general A/B to STB correction, rather Panoramix to Gir tek comparison.

and second off...?

Also, isn't any tek that goes from acid soak to basifying A/B? People seem to get hung up on the filtering, but it seems, at least to my mind, that if your extraction has an acidifying phase preceding a basifying stage then you're doing an A/B. I know some people don't consider the BLAB an A/B either, but again, I think it qualifies. I'd be interested in hearing from those who disagree as to why they feel this is not the case.

That is what I have always understood to be an A/b as well. However, as stated above, I am not a chemist, so I will leave the defining and qualifying to those more refined and qualified!

JBArk

 

[jbark]

Here are the results for STB pulls 1,2 & 3. (pics below). I also included a photo of the translucent "puddle" (its actually dry) surrounding the crystals. Is it really plant lipids - its colourless!?

I scraped the pyrex dish with a razor (pictured) A lot of it came off goopy, resinous... (after pouring off the naptha, it sat evapping for 30 hours, so I don't think this is due to residual naptha) I suppose I am going to need to clean and re-x... Is this standard for an STB?

The yield so far is 0.819 G from pulls 1,2 & 3.

Cheers,

JBArk

 

[endlessness]

As for the whole "is this an A/B?" discussion: I think if we are technical about it, then Snozz is right, in that there IS an acid soak before adding the base therefore one could theoretically call A/B. But I lean more towards Trickster's way of defining it, because the typical A/B's involve the characterizing filtering step. I think its better that we are more 'practical' about the definition and less strictly technical, otherwise cases such as Trickster's microwave example or some other more complicated apparatus might be called A/Bs but it will actually be misleading in the discussions. The same for the topic, I agree with Trickster's suggestion of changing the name to Panoramix vs Gir tek comparison or something of the sort (which is still very interesting of course, but just so people are not misled thinking results can be generalized between a typical A/B and an STB). Maybe we need a new category in the wiki such as 'pre-acid soak STBs' ?

By the way, jbark, that in the STB jars is definitely an emulsion, there is no such thing as 'general gunk' that sits on top of the mimosa. All the polar layer should be together and all the non-polar should be on top neatly separated, this third middle layer is an emulsion. So you can add more lye or pure salt and break it up, as some (maybe little but definitely some) of your solvent will be trapped there.

Those crystals look good already! The yellow could be plant oils, as mentioned, but it could also be a bit of n-oxide formed. I guess we would only know with some analytical equipment, but either way if you put it all together, its smokable Personally I would suggest maybe redissolving the crystals gotten from naphtha-based extractions in acetone or alcohol/IPA, and evapping again, or letting it air dry for long, just to make sure there isnt any naphtha traces on them.

Anyways, im very curious of the final yields and pictures! Good work so far, jbark! If you want, you can recrystalize that STB stuff. It does happen at times that it is like that, other times its more pure white, or it can be even yellower, it really depends on all the many variables as well as the mood of the gods

and do look into limonene extractions one day, I seriously love them and Im sure you will too

 

[Gir]

I find it normal to clean my crystals whether or not I use stb or a/b.

I usually separate the hard chunky's from the powder, and re-x the powder, save the chunkies, I put them in joints, its easier to have a chunky in there and have it melt all down the joint, then powder everywhere imho. I dont wannafightaboutit.

By the way, jbark, that in the STB jars is definitely an emulsion, there is no such thing as 'general gunk' that sits on top of the mimosa. All the polar layer should be together and all the non-polar should be on top neatly separated, this third middle layer is an emulsion. So you can add more lye or pure salt and break it up, as some (maybe little but definitely some) of your solvent will be trapped there.

HAH! Dont doubt my POWAH Again!!! (just kiddin bud) I know those emulsions when I see 'em. If its not already completely gone (which I believe it might be) you can set it on something that vibrates..(my motorcycle works wonders) and add some non-iodized salt, it will separate faster.

btw: that is my scale.. thank you for making it look ridiculously clean, can I have it back now?



-gir

 

[gibran2]

If we think about an A/B in terms of the necessity of an acid phase, then I think the definition of what an A/B really is becomes clearer. The only reasons I can think of that necessitate having DMT in a heat-stable, water-soluble form (salt) are boiling and filtering.

Boiling may be done to break down whole bark, or at a later stage to reduce liquid volume. If a solution containing freebase were boiled, much of the DMT would be lost.

Filtration may be done to separate DMT in solution from MHRB solids. DMT freebase is not soluble in pH-neutral or basic water, so much of the DMT would remain with the solids if freebase were filtered.

So, if high heat isn’t going to be applied and filtration isn’t going to be performed, then there’s no reason I can see for acidifying. Some TEKs acidify and then immediately basify without any intervening boiling or filtering. Unnecessary! (And not an A/B in my book.)

 

[prottel]

I also included a photo of the translucent "puddle" (its actually dry) surrounding the crystals. Is it really plant lipids - its colourless!?

I also get that translucent goop on the bottom of the glass. Not sure how to remove it.

 

[gibran2]

I also included a photo of the translucent "puddle" (its actually dry) surrounding the crystals. Is it really plant lipids - its colourless!?

I also get that translucent goop on the bottom of the glass. Not sure how to remove it.

I’m fairly certain that’s DMT that didn’t crystallize. It will dry out and form a yellowish-white solid.

 

[jbark]

Endlessness wrote:

By the way, jbark, that in the STB jars is definitely an emulsion, there is no such thing as 'general gunk' that sits on top of the mimosa. All the polar layer should be together and all the non-polar should be on top neatly separated, this third middle layer is an emulsion. So you can add more lye or pure salt and break it up, as some (maybe little but definitely some) of your solvent will be trapped there.

I thought "general gunk" was accepted scientific terminology - i have been misled!!

I added 1 heaping tsp full of NaOH to each of the mason jars. An hour later, It is even cloudier, with the "general gunk extending into the layer of naptha!! If it doesn't settle in a couple more hours, i'll add more NaOH and post pics.

and do look into limonene extractions one day, I seriously love them and Im sure you will too Very happy

Next on the list!!

Insofar as the A/B vs STB controversy goes, I am given to understanding that if no filtering and/or boiling is involved, then it is not an A/B. A subcategory is definitely required, if this is the case. As stated elsewhere, my methodology was to choose to teks that were more or less equal in their simplicity. In the absence of workable definitions, I simply routed through the lists of A/B and STB teks on the wiki. How about posting clear definitions of what constitutes these particular tek types, cleaning up the existing lists and creating one or more subcategories to accommodate the "inbetweens"?

Thanks for your feedback Endlessness. Always appreciated.

JBArk

 

[endlessness]

So, if high heat isn’t going to be applied and filtration isn’t going to be performed, then there’s no reason I can see for acidifying. Some TEKs acidify and then immediately basify without any intervening boiling or filtering. Unnecessary! (And not an A/B in my book.)

yes you have a good point.. I was also pretty skeptical of the necessity of a plain acid soak specially the quick ones and for prepowdered bark. If its very long soak and for bark in pieces, then maybe yes it could make some difference. But in any case, we can only really know if it makes a difference or not by doing side-by-side tests

 

[jbark]

But in any case, we can only really know if it makes a difference or not by doing side-by-side tests

Exactly!!8)

JBArk the pioneer closet chemist!

 

[jbark]

HAH! Dont doubt my POWAH Again!!! (just kiddin bud) I know those emulsions when I see 'em. If its not already completely gone (which I believe it might be) you can set it on something that vibrates..(my motorcycle works wonders) and add some non-iodized salt, it will separate faster.

btw: that is my scale.. thank you for making it look ridiculously clean, can I have it back now?



-gir

I bowah down befowa yo POWAH.

I have added lye and crossed the old fingers. I don't have a motorcycle, so I might balance it on the GF's vibrator after that, but I don't know if the batteries will last long enough!!8)

As for your scale - he who sweeps, sweeps for keeps my friend!!

JBArk

 

[Trickster]

So, if high heat isn’t going to be applied and filtration isn’t going to be performed, then there’s no reason I can see for acidifying. Some TEKs acidify and then immediately basify without any intervening boiling or filtering. Unnecessary! (And not an A/B in my book.)

yes you have a good point.. I was also pretty skeptical of the necessity of a plain acid soak specially the quick ones and for prepowdered bark. If its very long soak and for bark in pieces, then maybe yes it could make some difference. But in any case, we can only really know if it makes a difference or not by doing side-by-side tests

Actually swim did a similar comparison but between PanoraMIX's tek and an A/B. Not exactly side-by-side as in simultaneously, but pretty close to it. Same batch of prepowdered mhrb (50 g), same lab quality chemicals (distilled vinegar, heptane, etc). Swim doesn't think that doing the acid part in an extractor makes any difference. Its the same acidified boiling water wash.

Before crossing Panoramix's off the list swim ran it three times. Each time yields were not spectacular, quite possibly because of lots of spice cleaning during which losses are inevitable. On the average PanoraMIX's yields were below 1%.

On the other hand decanting, filtering and defatting of acidified aqueous phase in an A/B do not lead to such losses, or so it seems. Swim does not follow a particular A/B tek, but it is pretty simple and straightforward.

1. Acidified water extraction.
2. Thorough decanting and filtering
3. Defatting with heptane.
4. Basification to pH~12.5 with NaOH.
5. 5-6 pulls with 20 ml of heptane each.
6. Reduction of combined pulls.
7. Freeze-precipitaion.

She did the above tek more than 3 times already and yields on the same batch and the same mhrb quantity were consistently higher (1.3% - 1.4%). Someday she plans to skip the defatting stage out of curiosity to see if it is really necessary.

Of course the above is not a rigorous scientific experiment, just a personal observation.

 

[jbark]

Trickster - it was the defatting in QT's tek that was the time killer - added almost 10 days to the extraction!! The filtering takes time, too - that's why I chose Panoramix (and perhaps consequently disqualified the test as a true A/B vs STB). Oh well, I'm sure the comparison will still be useful. It will be at the very least for me - i am in search of the simplest, most efficient and safest tek (safe in terms of toxicity of final product). Still have to experiment with the foodsafe route. That'll be next.

JBArk

 

[Trickster]

Trickster - it was the defatting in QT's tek that was the time killer - added almost 10 days to the extraction!!

10 days :shock: ? I didn't try the QT tek, but for me defatting is the fastest part of the process. Takes about 20 min.

The filtering takes time, too

It takes two hours at most for me. Don't know, maybe because I do not extract more than 100 g at a time (usually 50 g). And maybe because I am dealing with less than 0.5 l of acidified water.

I'm sure the comparison will still be useful. It will be at the very least for me

I am sure it will, as mine was for me.

Sorry if I offended you in any way.

- i am in search of the simplest, most efficient and safest tek (safe in terms of toxicity of final product).

I believe everybody on this forum is looking for the same.

 

[jbark]

Trickster - it was the defatting in QT's tek that was the time killer - added almost 10 days to the extraction!!

10 days :shock: ? I didn't try the QT tek, but for me defatting is the fastest part of the process. Takes about 20 min.

The filtering takes time, too

It takes two hours at most for me. Don't know, maybe because I do not extract more than 100 g at a time (usually 50 g). And maybe because I am dealing with less than 0.5 l of acidified water.

I'm sure the comparison will still be useful. It will be at the very least for me

I am sure it will, as mine was for me.

Sorry if I offended you in any way.

- i am in search of the simplest, most efficient and safest tek (safe in terms of toxicity of final product).

I believe everybody on this forum is looking for the same.

The 10 days was for defatting was because you are required (if memory serves) to defat 3x, with at 48-72 hours soak time between. Also a huge waste of naptha... Same with the filtration - filter, keep mhrb juice aside, resoak filtered mhrb powder in acid for 24-48 hours X 3...:shock:

You can see why I am looking for a quicker tek!

No worries though Trickster, it takes a lot more than that to offend me!! But your initial post was curt, to say the least...

JBArk

 

[endlessness]

I've always felt defat to be such a huge waste of solvent, sooo inneficient for cleaning. Since fumaric acid methods came up, where none of the fats will anyways be precipitated, I look at defatting as an outdated technique. But even without fumaric acid, plain recrystalization is just soooo much more efficient and the yield loss is not much if you do a second small pull on the gunk left behind when recrystalizing. When I used to go for naphtha-based teks, I would get 1+% even after recrystalizing, pure stuff, no issues, no huge waste of defatting solvents..

But yeah, limonene teks is the way to go IMO. Yields are superb and one can even get pure white crystals too, with a couple of extra steps, as one can see in the now updated BLAB tek.

Anyways, jbark, still curious of the results

 

[Rivea]

All,

I think this is a great discussion from which I can take ideas and try myself. Also I developed this tech with the help of Trickster in a long series of private messages that I did want to share with you all...

In my tech below I always use Reverse Osmosis (RO) filtered tap water. I measured the total dissolved solids at 10 ppm... not exactly distilled, but pretty clean and chlorine free. The PH is approximately 5.8 which is typical for steam distilled water, and for USP water for infusion that I buy from B. Braun for IV work.

This last week I just finished a classical A/B using 100 powdered MHRB, acetic acid, lye, and 35/60 petroleum ether. I did three acid extractions on an overnight simmer while I was sleeping. Then I decanted each pull by drawing out the liquid using a syringe with at rigid tube attached to it after each pull settled in the refrigerator over night. I did two decanting operations on each acid pull. The first acid pull required almost no filtration.

The second pull was much cloudier, so I set it aside. The third pull was more cloudy with lots of fine particulates even after vacuum filtration, but this is because I pressed all the juice from the MHRB mush before discarding it. Doing the acid step as proposed by gibran2 in post #9 would make life even easier and my kitchen smell better and greatly reducing the time for acid extraction. It would also reduce the lye required for subsequent basification which would be good as well. Perhaps cold processing would also completely negate any reason to defat the acidifed solution as well.

I kept separate the first pull from the 2nd/3rd acid pulls to make more manageable amounts of fluids for my glassware. I reduced each separately down to approximately 180 ml, and then defatted each in a 250 ml separation funnel three times using 30 ml PE each time. The first acid pull had a slight emulsion that took a few hours to resolve on the first defat. The second and third defat ops on this pull took about 15 minutes total. The defat operations on the subsequent acid solution was nasty. I wasted some PE because of over shaking, but I'll live.

Once I had the acid solutions defatted, I measured the PH and it was about 2.2. I processed each acid pull identically and at this stage there appeared to be no differences in the results which I did on two nights. I took 150 ml of water and added 18 grams of Na-OH to it slowly stirring it constantly until fully dissolved. Then I slowly mixed this into a beaker containing the acid solution until the PH was about 12.8 constantly stirring. When basified I had about 275 ml of solution.

I poured this into my 500 ml separation funnel and did 7 gently warmed pulls using 35/60 petroleum ether. I used 35 ml 4 times and used 20 ml 3 times... probably overkill to the max. Because of the volatility of the 35/60 PE, I lost a lot to evaporation and ended up with about 140 ml of PE laden with spice. I had to be very careful to vent my separation funnel very frequently. One time the glass stopper actually popped out like a Champaign cork and dropped into the sink over which I was working. Scared the crap out of me in the silence of 2AM.

To facilitate the freeze precipitation and to help conserve PE, I distilled this and recovered approximately 100 ml of PE leaving about 40 ml laden with spice. The spice laden PE had that VERY distinct plasticine aroma.

I freeze precipitated the spice from the PE in a sealed covered Pyrex container. The first batch I let sit in the freezer (-20 deg F) over night. The second I let sit for two hours. Then I took the container out of the freezer, dumped the PE into another bowl, and put the cover back on the bowl. I warmed the bowl under running water until it was warm to the touch, uncovered it and let any remaining PE evaporate with the cool air from a fan to assist. After all smelled clean, I scraped the crystals from the bowl into a 100 mm Petri dish, chopped them to allow the un-evaporated PE to escape, and then weighed it at 0.5 grams.

The second freeze precipitation batch I only left in the freezer for two hours. I did the same as above to remove the spice. However I put the bowl containing the PE back into the freezer to see if more would precipitate out. It did not. In fact, evaporating all of the PE from the second bowl resulted in a slight haze of spice on the bowl which is an insignificant amount. After drying the crystals from the second batch they weighed in at 0.5 grams.

The total yield was 1.0 grams which amounts to exactly 1.0%. It is non oily, completely white without a hint of any other coloration. I plan to process some of it further into fumarate form making it as clean as possible, sterile, and isotonic.

Perhaps this is all overkill, but I am kind of a perfectionist for good reason.