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A/B vs STB Side By Side


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#1 Phineas_Carmichael

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Posted 02 May 2010 - 09:31 AM

Side by Side A/B vs. STB Methods and Materials

I. Equipment


1. Assorted Glassware or HDPE
2. 1L Sep Funnel
3. Digital pH meter
4. 500mL Vacuum Filtration Apparatus
5. Personal Protective Gear

II. Chemicals


1. Distilled H2O
2. 37% Muriatic Acid
3. Crystalline Sodium Hydroxide (Lye)
4. Crystalline Sodium Carbonate (Soda Ash)
5. VM&P Naphtha

III. A/B process


1. 100g MHRB will be gently simmered in 250mL pH 4 HCl solution for 30 minutes and allowed to cool for 30 minutes. The tea will be filtered with vacuum, the filtrate saved and set aside. The Filtrand will be returned to 250mL pH 4 HCL to be boiled again, repeating the step 5 times.
2. Filtrand will be simmered once in 250mL D-H2O, filtered and discarded.
3. Combined filtrate pH will be adjusted to pH 4 with HCl
4. 200mL Naphtha will be added to the combined filtrate, stirred gently for 15min, and discarded. [Repeat 2x]
5. The remaining acidic solution will be reduced to 400mL with a gentle simmer
6. Solution will be basified to pH 12 with concentrated Sodium Hydroxide Solution [If necessary, will be reduced to 800mL by evaporation]
7. 200mL Naphtha will be added to the base, stirred gently for 15 minutes, separated and retained [Repeat 2x]
8. Resulting 600mL Naphtha will be washed

A. 1x 100mL pH 10 Sodium Carbonate Solution
B. 2x 100mL d-H2O

9. Washed Naphtha will be reduced to 300mL by evaporation and frozen for 48 hours
10. Remaining naphtha will be poured off crystals and saved for a rainy day
11. Crystals will be allowed to dry completely before weighing and bottling.

 

IV. STB Process


1. 100g Sodium Hydroxide will be added to 700mL d-H2O
2. 100g MHRB will be added to this solution, mixed well and allowed to sit for 2 hours
3. 200mL Naphtha will be added to the base, stirred gently for 15 minutes, separated and retained [Repeat 2x]
4. Resulting 600mL Naphtha will be washed

A. 1x pH 10 Sodium Carbonate Solution
B. 2x d-H2O

5. Washed Naphtha will be reduced to 300mL by evaporation and frozen for 48 hours
6. Remaining naphtha will be poured off crystals and saved for a rainy day
7. Crystals will be allowed to dry completely before weighing and bottling.

 

V. Hypothesis


A/B extractions yield larger amounts of higher purity product. They are chemically more efficient than STB extractions, and require only a further investment of the chemist's time, at most tripling the time required for an extraction.

VI. Prediction


1. If A/B extractions are more efficient than STB, then performing an A/B with identical stock solutions, solvents, and botanicals will yield a larger amount of higher purity product.
2. Working with 100g MHRB will probably not conclusively show higher efficiency in A/B extractions. However, a recrystallization may be undertaken on the STB spice in an attempt to purify it to a point visually comparable to the A/B extract. The respective weights of these samples I am certain will show that A/B extractions yield higher quantities of more pure DMT than STB extractions.

=============
Freddy is awaiting a shipment of botanicals and intends to document the testing of this hypothesis within 2 weeks.
Questions for Topiates:

1. Is the extraction procedure correct for both types of extractions?
2. Has Freddy overlooked any step in the procedures?
3. Your predictions regarding the hypothesis, accept or reject?
4. Will this experimental design accurately show which extraction is more efficient?
5. Discuss.


Edited by wharfrat, 19 June 2016 - 04:01 PM.

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#2 Mr Kush

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Posted 02 May 2010 - 10:03 AM

I have done both plenty of times, my experimentation deffently matches with your hypothesis. when aiming for high quality a/b's always take the win for better yeild. I have tried cleaning stb quality dmt by rexing with naptha/heptane, FASA precipitation, polar wash, and with activated carbon. In the end once purified through any of these methods the ending weight was not as good as what I would have yeilded doing a proper a/b.

Remember tho an a/b has WAY more variables tho then does a standard stb, thus the results can be hard to accuratly calculate, and thus is why I say if the a/b is done proper the results are much better.

I like where this is going tho, I havent seen anyone do them back to back with good descripitions of each process.

You seem to have the process down quite well but imo there is room for improvment. for starters on the a/b you might want to use alittle more dh20 to do your acid soaks with, acetic acid has better properties to be used with nn-dmt then does hci, the ph ranges could be adjusted (nn-dmt has a pk of 8.68), if you can doccument the temperatures of each solvent during the process that would be amazing as that makes a HUGE difference. To be fair with the stb I would say soak the mhrb in the basified solution for atleast 12-24 hours before adding the NP solvent as I dont think all the cell walls will be broken down in 2 hours....atleast this is what I have found in my experimentation.

Good luck! cant wait to see the results:rasta:.

#3 McDozd

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Posted 02 May 2010 - 10:08 AM

I dont think all the cell walls will be broken down in 2 hours


SWIM have had no problems with that if the MHRB is down to powder and fibers. SWIM usually waits around 2 hours with the mixture in a 140sh heat bath. Then preforms the pulls with ease.
:amazed:

#4 Mr Kush

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Posted 02 May 2010 - 10:48 AM

well, Honestly I have noticed a defference IME.
for clarification I always used galactic toads mhrb AS IS.
I have been using his material far before he became a sponsor and before I was a member here.
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#5 McDozd

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Posted 02 May 2010 - 11:15 AM

Ok. Let me clarify. FOAF has gotten bark from ebay tons of times. Always powdery and dry. So, breaks down fast. FOAF has recently got some of the TOADS bark last batch and the yeild increase was almost a whole percent and quality way better. FOAF attributes this to the bark that was still a little fibery and was still moist! FOAF def recommends our sponsers bark as shipping it non-expedited was reasonable price and 3 days to arrive. :headbang:
Anyway, the FOAF said the fresh fibery bark still broke down well in 2 hours, BUT... He got another 1.1 on 5th pull! So it is possible that it all hadnt broke down he is not sure. Total net after drying off 2lbs was 18.2 :eusa_clap

#6 bbd2

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Posted 02 May 2010 - 11:27 AM

[SIZE="3"]
...

1. 100g MHRB will be gently simmered in 250mL pH 4 HCl solution for 30 minutes and allowed to cool for 30 minutes. The tea will be filtered with vacuum, the filtrate saved and set aside. The Filtrand will be returned to 250mL pH 4 HCL to be boiled again, repeating the step 5 times.

...

Questions for Topiates:
[indent=1]1. Is the extraction procedure correct for both types of extractions?

...

4. Will this experimental design accurately show which extraction is more efficient?
5. Discuss.


i think you will need to use more water here
a cup of water sounds too low
id estimate you will need at least 400 ml

everything else sounds good

looking forward to seeing what you find
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#7 Phineas_Carmichael

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Posted 02 May 2010 - 11:35 AM

I like where this is going tho, I havent seen anyone do them back to back with good descripitions of each process.

That's the idea, I haven't seen it either and am mad curious.

You seem to have the process down quite well but imo there is room for improvment. 1)for starters on the a/b you might want to use alittle more dh20 to do your acid soaks with, 2)acetic acid has better properties to be used with nn-dmt then does hci, 3)the ph ranges could be adjusted (nn-dmt has a pk of 8.68), 4)if you can doccument the temperatures of each solvent during the process that would be amazing as that makes a HUGE difference.

1) I thought 250mL seemed low, 500mL is probably a better amount. Just trying to cut corners :spank: and reduce evaporation time.
2) Is acetic acid preferred because of some property of the acetate vs hcl salt? Rephrased: What properties make acetic preferable to hcl?
3) nn-dmt's pk of 8.68: Does this mean that the ideal pH for the basic phase is around 9? Rephrased: Got any good resources that explain pK values as they relate to extractions?
4) Solution temperatures can easily be recorded throughout the experiment. Didn't think of that! :eusa_clap

To be fair with the stb I would say soak the mhrb in the basified solution for atleast 12-24 hours before adding the NP solvent as I dont think all the cell walls will be broken down in 2 hours....atleast this is what I have found in my experimentation.

Makes sense. The STB can easily be prepared first and set aside while the A/B is carried out.

Good luck! cant wait to see the results:rasta:.

Many thanks for your thoughts. Freddy wants to have the process nailed down and solid in his brain before he begins.

Ok. Let me clarify. FOAF has gotten bark from ebay tons of times. Always powdery and dry. So, breaks down fast. FOAF has recently got some of the TOADS bark last batch and the yeild increase was almost a whole percent and quality way better. FOAF attributes this to the bark that was still a little fibery and was still moist! FOAF def recommends our sponsers bark as shipping it non-expedited was reasonable price and 3 days to arrive. :headbang:

Someone correct me if I'm wrong, but I believe a key factor in STB tek development was the scarcity of powdered bark in the early days, and the PITA factor of powdering it yourself. Looking at "pioneer" STB teks, shredded rootbark is usually used and the fact that it needn't be powdered as in an A/B is greatly emphasized. Interesting that GalacticToad's bark was so fresh, probably contributes to the high yields people have been getting. Glad he's around! :loveeyes:

Anyway, the FOAF said the fresh fibery bark still broke down well in 2 hours, BUT... He got another 1.1 on 5th pull! So it is possible that it all hadnt broke down he is not sure. Total net after drying off 2lbs was 18.2 :eusa_clap

What the hell is your FOAF going to do with 18.2g? :headbang: I'd wager a toe (but not a testicle) that if he had waited more than 2 hours on the soak that same 18.2g would have come out, but in fewer pulls.
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#8 McDozd

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Posted 02 May 2010 - 11:41 AM

What the hell is your FOAF going to do with 18.2g? I'd wager a toe (but not a testicle) that if he had waited more than 2 hours on the soak that same 18.2g would have come out, but in fewer pulls.

You are probably right. FOAF sometimes hurrys things, but as long as he doesn't get lye-locked, he will pull a 5th time to make sure he gets it all.
:rasta:

#9 BioTron

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Posted 02 May 2010 - 11:55 AM

If you are going to do the initial acid extraction 5 times, you should use 5 repetitions as your standard. Do 5 naptha pulls of a smaller quantity instead of 2 pulls with a larger quantity. Another variable is you are boiling your acid/bark in the A/B but you aren't boiling the MHRB with the STB procedure. If you boil one, boil the other. Keep all conditions the same from A/B to STB.

#10 BioTron

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Posted 02 May 2010 - 12:00 PM

On pka's: If nn-dmt has a pka of 8.68, that basically means that when placed in a ph solution of 10.68 there is not a significant quantity of dmt left as an acid, meaning it is essentially all frebase. When you acidify a solution of dmt to ph 6.68, there is not a significant quantity of dmt left in freebase form, meaning it has all been converted to the desired acid form.

Why is acetic acid better, IDK. I'd like to hear some more on this one too.

#11 Phineas_Carmichael

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Posted 02 May 2010 - 12:19 PM

If you are going to do the initial acid extraction 5 times, you should use 5 repetitions as your standard. Do 5 naptha pulls of a smaller quantity instead of 2 [actually 3, initial step + repeat 2x -P] pulls with a larger quantity.

That can be arranged and is logical. Thank you.

Another variable is you are boiling your acid/bark in the A/B but you aren't boiling the MHRB with the STB procedure. If you boil one, boil the other. Keep all conditions the same from A/B to STB.

My issue with this is that freebase nn-DMT(in suspension in basic solution) boils at 60-80C. If the basic solution is boiled [100C], the freebase in suspension will surely be damaged, won't it? I can't find data on DMT Acetate's boiling point, but I'm fairly certain it is higher that 100C and as such will not be damaged by boiling. Furthermore, STB teks don't call for boiling...

On pka's: If nn-dmt has a pka of 8.68, that basically means that when placed in a ph solution of 10.68 there is not a significant quantity of dmt left as an acid,[salt -P] meaning it is essentially all frebase. When you acidify a solution of dmt to ph 6.68, there is not a significant quantity of dmt left in freebase form, meaning it has all been converted to the desired acid[salt -P] form.

Thanks for this too. A +or- 2 difference between pKa and pH ensures that 99% of the desired compound is in suspension. This predicts an ideal pH of ~6 for the acid phase and ~11 for the basic phase, no?
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#12 McDozd

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Posted 02 May 2010 - 12:19 PM

Very good point BIO. Use should make the test fairly uniform so that the results are more definitive. I am interested in the difference in quality and yield. :)

Good luck with your experiment!
:rasta:

#13 whatchamacallit

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Posted 02 May 2010 - 01:40 PM

Don't boil the solution when it has DMT freebase. It can be boiled while in a salt form, but don't do it when in freebase form.

Those pH measurements will be okay for an a/b, but in an STB containing bark, emulsions would take forever to settle out. Also, many low yields have been attributed to using too little lye, so even if you do go at precisely those pH's, then save everything to add more lye later, to see if you can still get more yield from higher pH's.

Lower pH's in the acid soak phase of an a/b will also pull out more gunk, so measuring the pH at 6 should allow for cleaner DMT, but it also may take more soaks to get it all out. Again, saving everything until the end, may allow you to go back and find which steps could be done more efficiently in each process. Please take very detailed and specific notes of every step.

Also, acetic acid is nice to use because it evaporates off when reducing (leaving the pH stable), I believe, while the HCl concentrates, until it becomes concentrated enough to start to form a gas. I believe the best acid to use for getting the cleanest extract is ascorbic acid, and I would recommend it for the a/b (anecdotal evidence only).

This should be an interesting experiment.

#14 BioTron

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Posted 02 May 2010 - 04:35 PM

I should have known better and looked up the BP of nn-dmt as a freebase, oops. I do believe that you are correct, whatcha, about the HCl concentrating when reducing, but I still think that HCl would be a better choice as it completely dissociates and you will get by with using less of it to acidify than if you were using ascorbic or acetic. But you will be reducing the volume after the conversion to the acid salt, so ascorbic or acetic my very well work better. I love contradicting myself.

#15 Norman

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Posted 02 May 2010 - 05:35 PM

Looks good to me. I'd skip the NP wash though.

#16 McDozd

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Posted 02 May 2010 - 07:49 PM

All you a/b mad alchemist's out there.. don't you use white wine vinegar(5%)? I thought muratic didn't work as well as the WWV. The only a/b I have done used the WWV and I got a 1.8sh % yeild and it was off white to yellow. No dark tints to it what so ever. I can get just as good of a yield from a STB, and get what I think is just as good as the a/b just a little more yellow. Thats why I prefer STB to a/b, less work and almost as good outcome. Curious to see how your expiriment goes Phin.
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#17 eastwood

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Posted 02 May 2010 - 08:01 PM

Great discussion :hippie:

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#18 Norman

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Posted 02 May 2010 - 08:21 PM

All you a/b mad alchemist's out there.. don't you use white wine vinegar(5%)? I thought muratic didn't work as well as the WWV.


I used to use distilled white vinegar and then I switched to phosphoric acid. Muriatic has never worked that well for me, but I've heard of others having good luck.

#19 Phineas_Carmichael

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Posted 02 May 2010 - 09:09 PM

Lower pH's in the acid soak phase of an a/b will also pull out more gunk, so measuring the pH at 6 should allow for cleaner DMT, but it also may take more soaks to get it all out. Again, saving everything until the end, may allow you to go back and find which steps could be done more efficiently in each process. Please take very detailed and specific notes of every step.

Rest assured, notes will be taken :)

Also, acetic acid is nice to use because it evaporates off when reducing (leaving the pH stable), I believe, while the HCl concentrates, until it becomes concentrated enough to start to form a gas.

Good point in acetic acid's favor. In Freddy's last A/B, carried out with HCl, the pH of the acidic solution was lower after reduction. Should be easy to confirm by reducing acetic and hcl solutions by identical factors and recording before and after pH levels. Leaning towards changing the acid to a solution made with glacial acetic acid and d-H2O.

I believe the best acid to use for getting the cleanest extract is ascorbic acid, and I would recommend it for the a/b (anecdotal evidence only).

Let's let Freddy do this experiment first, and afterwards maybe he'll do something similar comparing different acids in the acid phase...

This should be an interesting experiment.

Thanks. Freddy's sure looking forward to it! :teeth:

Looks good to me. I'd skip the NP wash though.

To clarify, you mean step III. 4. where the acidic solution is combined with naphtha[defat] don't you?

All you a/b mad alchemist's out there.. don't you use white wine vinegar(5%)? I thought muratic didn't work as well as the WWV.

Vinegar is basically acetic acid solution that has been created as a waste product by an anaerobic bacteria. The 5% refers to the fact that the vinegar you buy is 5% acetic acid by weight. Another point in acetic acid's favor. Vinegar has "plant stuffs" in it though, if acetic is used, it will be as a solution created with glacial acetic acid and d-H2O in the interest of eliminating variables.

The only a/b I have done used the WWV and I got a 1.8sh % yeild and it was off white to yellow. No dark tints to it what so ever. I can get just as good of a yield from a STB, and get what I think is just as good as the a/b just a little more yellow. Thats why I prefer STB to a/b, less work and almost as good outcome.

That's more or less in line with what we've read. STB's are less work, for similar yields of more colorful products. Freddy has a bit of the "Walter White Syndrome," you know? Producing a snow white crystal is as much, if not more, of a thrill for him as smoking said crystal.
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#20 McDozd

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Posted 03 May 2010 - 08:06 PM

Good read Phin. Still waiting on Freddy's yield and quality differences. :loveeyes:
Anyway rock on, FOAF will always be a STB addict do to the simplicity and the little bit of color is nice. FOAFs is light yellow popcorn nugs. Extremely potent.
:teeth:




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