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Revisiting Loki's Tek - Extraction Troubleshooting


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#1 jeff

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Posted 05 November 2006 - 01:45 AM

Howdy all,

About a year ago, SWIM did a Mars tek MHRB extraction. Got decent yield, but the product was very harsh to smoke. Since other DMT SWIM had tried wasn't nearly as harsh, this was attributed to residual NaOH (despite using Na2CO3 + H20 followed by H20 solvent washes and freeze precip).

Recently she decided to try again using something closer to Loki's tek:

http://mycotopia.net...achmentid=17477
(this link to the pdf should work)

Things that seem good about this tek:
. Tannin removal / oxidative protection via vitamin C.
Granted this was apparently more important for Loki, working primarily with Acacia, than for someone like SWIM using MHRB. But it seems like such a nice idea.
. Boils down aqueous phase making entire extraction easier to handle (smaller amount of liquid).

Drawbacks to the tek:
. Expected yield isn't given.
. Amount of base to add isn't precalculated. Instead, we are to add NaHCO2 until foaming stops, then add NaOH until solution turns black.
Well what's black (especially considering it's opaque before starting to basify)? And, has anyone found a pH meter that's worth a damn? Papers don't seem to work on opaque, tarry solutions, and the digital ones SWIM has been able to get don't inspire much faith.

Anyway, there's enough detail missing from this tek that someone like SWIM could screw it up. I thought I'd share the details of SWIM's misadventures in hope that someone could help SWIM figure out what went wrong. Even if SWIM goes back to Mars' tek, figuring out what happenned is essential to her peace of mind!

The Plan:
Calcium ascorbate is used to acidify H20, which is used to extract very finely ground MHRB. Solution filtered, boiled down about 8:1, defatted 1X with Xylene. Solvent added (Bestine) and solution basified with bicarb until foaming stops, then lye until black. Solvent decanted off, washed with 10% Ammonia, dried with anhydrous MgSO4, then evaporated.*

* Evap is faster than precip, and yields bigger crystals. Everyone seems to recommend precip, but if your product is pure why not evap? The product can be still cleaned with recrystalization -- at least you know you got it all.

What seemed to go wrong:
Loki does not mix solvent into aqueous phase while basifying, but SWIM was worried this would not get as much product as stirring it in. Apparently a terrible idea. Adding NaHCO3 created foam that wouldn't go back into solution (about 1 part out of 5). Then, adding lye turned entire beaker to thick, grey foam that would not resolve. After waiting and waiting and heating foam with no change, SWIM decided to salvage the situation by boiling more Bestine on top of foam, and then by pouring foam from sep funnel through the same boiling Bestine, and then evaporating that Bestine.

Result:
Zero yield, of anything. Absolutely clean pyrex after 2 hours.

SWIM is pretty sure she didn't under-basify. Full lab notes in next message. Looking for ideas about what went wrong, as well as comments on the pros/cons of boiling down, vitamin C, evap, etc.

Thanks,

-Jeff
"Working to refine extractions even further!"

#2 jeff

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Posted 05 November 2006 - 02:08 AM

SWIM writes,

EXTRACTION
7pm- One metric fuckload MgSO4 ground in coffee grinder and placed in oven at 480deg F.

7:20- 4L dH20 set to boil. 50g Calcium Ascorbate USP added.

7:45- Solution boiling; 500mg finely-ground MHRB added. pH=4.3 according to digital meter.

8pm- MgSO4 broken and stirred, placed back into oven.
10g "Ascorbic acid" USP added to boiling solution. pH=3.9 according to digital meter.

8:30- MgSO4 re-ground and jarred.
Solution taken off boil.

8:50- Unknown quantity spilled on floor (< 8oz.).

9:40- Solution filtered (t-shirt) multiple times and put back to boil. MHRB discarded.

11:10- Solution taken off boil, poured into beaker. Volume = 350ml. 150ml dH20 added (total = 500ml). Placed in freezer.

12:15am- Decanted through cotton ball funnel into sep funnel (beaker was clean after decanting).

DEFAT
12:30- Added 50ml hot Xylene to sep funnel, turned. Waited 5min for layers to separate, discarded Xylene, placed solvent in beaker. Added 50ml hot Bestine.

1am- Sprinkled in NaHCO3, got thick foam. Stirred, then waited for foam to resolve. Repeated 2X. Finally beaker was 400ml solution, 100ml foam.

2am- Added ~7g NaOH (Red Devil) in 50ml warm dH20. Solution became homogenous grey foam.

2:15- Added 200ml warm bestine, put on hot plate, stirred. Thick emulsion formed. Heated in water bath.

4am- No change, heat turned off.

8:30am- 200ml of emulsion placed in separate beaker, to which 100ml Bestine was added. Heated on hot plate.

9:30am- Lots of foaming (bigger bubbles). 100ml sedement layer on bottom. Removed from heat. 3 layers obtained = 100ml sedement, 5ml black, 200ml dark brown foam. Placed in sep funnel, bottom two layers discarded = 200ml dark brown foam.

10am- Other beaker (~550ml) heated, 200ml Bestine poured on top, NOT STIRRED. 200ml DBF from sep funnel poured through Bestine. Beaker total 800ml. Heated.
Poured off 180ml clear Bestine and placed in sep funnel with 120ml fresh bestine = 300ml clear solvent.

WASH
11am- Added 40ml 10% NH4OH and shook. Removed 40ml NH4OH.
Stirred in 2 tsp. MgSO4, filtered out with coffee filter 3X.

11:20- Placed solvent in 2 pyrex casseroles, in front of fan.

1:30pm- Casseroles clean and dry.

-Jeff

#3 Guest_lost_onabbey_rd_*

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Posted 05 November 2006 - 02:25 AM

my FOAF says that you underbasifyed...
add more lye to the mixture till the grey foam turns into black oily stuff..
didn't read the whole post but a friend asked that i convey that message
lost

#4 marsofold

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Posted 05 November 2006 - 09:19 AM

No mention of vendor source. Hmmm...not researchbotanicals was it?

The Calcium Ascorbate. Something I've wanted to try to reduce tannins. And the Ascorbic Acid. Most people use 1-gram/liter of the ascorbic acid, but a bit more won't hurt since acidification is logarithmic. And since you measured the ph, all is probably well at this point.

You reduced from 4-Liters down to 350-milliliters. That is about an 11:1 ratio. Probably OK, but the highest reduction ratio I've read about that was confirmed from someone I knew online was 6:1. So I count that as an unknown factor.

The defat. OK. Done it myself many times for non-Mimosa sources of DMT.

"Added 50ml hot Bestine". Don't know if it really matters, but the non-polar is usually added AFTER basification.

Basification. You added an unspecified amount of Sodium Carbonate first, then added 7-grams of lye. Mistake. Not enough lye. The ascorbic acid, unlike vinegar (acetic acid), did not vaporize off when the solution was reduced to 350ml. So all of that ascorbic acid was still in there. And had to be neutralized before the ph would go above neutral(7). Which would require extra lye. Your continuing emulsion proves that the ph was too low.

"200ml Bestine poured on top, NOT STIRRED" Major mistake. The non-polar solvent must be very well mixed into the brew to absorb the DMT. Otherwise the interface between the two layers is the only exchange area involved. It's a surface area thing. That's why the jug I use to extract DMT is inverted upside-down rightside-up every one second for 5 minutes. The flow of the non-polar solvent through the brew maxes out the surface area so the DMT will move into it. This is a possible reason for the nil yield.

The wash. Adding ammonium hydroxide (at room temperature?) to the non-polar solvent. High-risk procedure relative to yield. Washes need to be done FAST. Did you drain off the ammonium hydroxide in SECONDS? Ammonium hydroxide has a ph of 11, just barely enough. Chilling the solution and quickly passing it over crystals slows the loss enough to make it efficient (90%). Speed is of the essence. Otherwise the freebase converts back to the salt and goes into the wash solution. And is lost.

As simple as most TEKs look, they are unforgiving on many factors. Deviate at your own risk. When I remember how much DMT I lost determining the optimum volume of ammonium hydroxide used for the wash, (sigh)...more than most people have ever extracted. Stick to the roadmaps and buy your rootbark from a respected vendor.

#5 jeff

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Posted 05 November 2006 - 03:50 PM

Hi Mars!

No mention of vendor source. Hmmm...not researchbotanicals was it?


SWIM has to look that up in her notes and get back to me. Will post later.

The Calcium Ascorbate. Something I've wanted to try to reduce tannins. And the Ascorbic Acid. Most people use 1-gram/liter of the ascorbic acid, but a bit more won't hurt since acidification is logarithmic. And since you measured the ph, all is probably well at this point.


Loki only calls for Calcium Ascorbate, but SWIM had Ascorbic Acid too and thought she'd add some to make sure the pH was no higher than 4.

You reduced from 4-Liters down to 350-milliliters. That is about an 11:1 ratio. Probably OK, but the highest reduction ratio I've read about that was confirmed from someone I knew online was 6:1. So I count that as an unknown factor.


SWIM menat to reduce to 500ml, but was taken by surprise at the rate of boil-off.

"Added 50ml hot Bestine". Don't know if it really matters, but the non-polar is usually added AFTER basification.


Oops, an error in the notes. SWIM did 1 defat with Xylene followed by 1 with Bestine. Solvents were removed before basifying.

However note that Loki, if I'm reading him right, calls for neutralizing the solution, then adding solvent on top and raising the pH to form the salt by pouring NaOH solution through the solvent layer! SWIM didn't trust this because your tek calls for mixing the solvent in well. But thinks Loki does it this way to prevent emulsions?? Would not mixing be OK because of the much higher concentration of product in the *reduced* extract vs. your tek? Loki doesn't give yields = makes it hard to compare teks.

Basification. You added an unspecified amount of Sodium Carbonate first,


Bicarb. No Na2CO3 was used in this extraction.

then added 7-grams of lye. Mistake. Not enough lye. The ascorbic acid, unlike vinegar (acetic acid), did not vaporize off when the solution was reduced to 350ml. So all of that ascorbic acid was still in there. And had to be neutralized before the ph would go above neutral(7). Which would require extra lye. Your continuing emulsion proves that the ph was too low.


Aha, of course! Thanks Mars! In subsequent message I will try to work out the amount of lye needed.

"200ml Bestine poured on top, NOT STIRRED" Major mistake. The non-polar solvent must be very well mixed into the brew to absorb the DMT.


In this case mixing in would have caused nonpolar to be lost in the emulsion.

Otherwise the interface between the two layers is the only exchange area involved. It's a surface area thing. That's why the jug I use to extract DMT is inverted upside-down rightside-up every one second for 5 minutes. The flow of the non-polar solvent through the brew maxes out the surface area so the DMT will move into it. This is a possible reason for the nil yield.


I wonder how Loki got it to work?

The wash. Adding ammonium hydroxide (at room temperature?)


Chilled.

to the non-polar solvent. High-risk procedure relative to yield. Washes need to be done FAST. Did you drain off the ammonium hydroxide in SECONDS?


Yes.

Ammonium hydroxide has a ph of 11


SWIM thought in any case it would be better than the dH20 wash that seemed to work for her with your tek.

Chilling the solution and quickly passing it over crystals slows the loss enough to make it efficient (90%). Speed is of the essence. Otherwise the freebase converts back to the salt and goes into the wash solution. And is lost.


The idea for using ammonia on the nonpolar came from this thread:

http://mycotopia.net...863<br /><br />In which fmoc seems to make a good argument for wet ammonia washing.

Stick to the roadmaps and buy your rootbark from a respected vendor.


SWIM is interested pushing the frontier a little bit. She understands losses are unavoidable when trying new things. She just wishes her chemistry were better!

-Jeff

#6 jeff

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Posted 05 November 2006 - 04:01 PM

re. source of MHRB, SWIM says it was bouncing bear.

re. pH, SWIM said she used an online pH calculator based on 50g of Calcium Ascorbate and got 5g NaOH, then used 7 to be safe. As for doing a calculation by hand, my chemistry isn't quite up to snuff. :(

-Jeff

#7 jeff

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Posted 05 November 2006 - 11:21 PM

re. source of MHRB, SWIM says it was bouncing bear.

re. pH, SWIM said she used an online pH calculator based on 50g of Calcium Ascorbate and got 5g NaOH, then used 7 to be safe. As for doing a calculation by hand, my chemistry isn't quite up to snuff. :(

-Jeff


Correction: SWIM says she assumed bicarb had neutralized solution, and caculated 5g of NaOH to bring the solution to 13.4, and then used 7g to be safe. -Jeff

#8 jeff

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Posted 05 November 2006 - 11:27 PM

Here are SWIM's notes:

I read that NaOH is 40g/mol. From

http://chemware.co.nz/vbsph.htm

I got that a pH of 13.4 from NaOH requires
0.251 mol/L. With 500ml of solution, that's

40 * 0.251 / 2 = 5g

which I added to 50ml warm dH20 and then to the
solution.

Perhaps the bicarb step didn't achieve a pH of 7....?

-Jeff

#9 marsofold

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Posted 06 November 2006 - 06:36 PM

You weren't too far off on the lye. And BBB's bark is generally respected for good yields. The lack of non-polar mixing or major wash losses were probably the main reasons for the poor yield.




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