A/B, MHRB, DCM [low yield]

[Shaolin]

Material: 100g MHRB (JimJamShop)
Boiling: 4*55 min boils, 1000ml each (4000ml total), reduced to 500ml

A: 3.8-4, acetic (white vinegar, 9%)/phosporic (phDown) ; both were used
B: 12.2, NaOH (Sigma)

Solvent: 4*25 DCM (Sigma)
1. pull - 100 mg
2. pull - 60 mg
3. pull - 100 mg
4. pull - 190 mg

DCM was left to evap for 48 hours and then scraped.

Problem ? Well DCM should pull a lot but even with four pulls I get a yield of only 0.45%.

I have not done a re-x (with heptane, T > 65C) but previous attempts showed that I can expect a return of about 10%, so 40-50mg. Fail.

 

[Infundibulum]

The whole procedure sounds fine. The low yield is either because of bark being just too weak (this is not unheard of) or something is wrongg in your procedure. It is easy to find out if you basify to a much higher pH e.g. (13-14) and pull with naphtha and or heptane. If still nothing, then blame bark.

It is hard to believe DCM pulls that little from pH 12. Xylene and limonene easily pull everything from pH 12. Have you checked the pH correctly? is the pH meter calibrated?

 

[endlessness]

yeah I found it pretty weird, was going over with him in the chatroom and just cant seem to pinpoint why. He says he checked pH with both papers and calibrated meter. Usually one could think bad bark, but the bark is from jimjamshop, consequently all coming from adenium, and in terms of yield I've personally never heard of any of their bark resulting in bad yields. Did you guys?

I mean, adenium powders these big quantities of mimosa root bark (and later divided in smaller batches for selling), so the bark quality is somehow "standardized", its hard to imagine that one particular small personal shipment to a person is bad quality while all the other bark adenium/jimjam is shipping is specially high yielding...

I really dont know what else could be the reason though...

Do you still have some of the bark, shao? or any possibility of getting new bark? Would be interestng to try another proceedure with same bark, and/or to try same proceedure with another bark..

 

[Noman]

Agitation maybe?
I'd base it up to 13.5 and shake the shit out of it and see.

 

[Trickster]

I would like to suggest a few obvious ideas:

First, I would exclude the bark quality variable.

1. Did you try different teks on this batch? Did they produce better yields?
2. If not, then try one. Say, do a straightforward A/B and pull with Heptane/Hexane instead of DCM. Do even more boilings then you usually do. Freeze/thaw the bark a few times to make sure that all cell walls are broken.

I did a few DCM extractions followed by Hexane/Heptane re-x and my results are more encouradging. I used a year-old batch of adenium powdered mhrb every time.

Before trying DCM I ran a number of different teks on this batch (Panoramix, IPA+A/B, Ethanol+A/B, Methanol+A/B). Excluding a few major screw-ups my yields averaged at 1%. So, when I started to experiment with DCM I was pretty sure that the bark contains at leas 1% of spice.

My DCM extractions, followed by Heptane/Hexane re-x, yielded 0.5% - 1.2%, that correlates with other teks.

P.S. I've stopped experimenting with DCM due to concerns re. unwanted products of reaction between DMT and DCM.

 

[Trickster]

Agitation maybe?
I'd base it up to 13.5 and shake the shit out of it and see.

It is a possibility. I noticed an increase of yields since I've started stirring my pulls with a magnetic stirrer for 10-15 min.

 

[soulfood]

As the 4th pull was the largest this looks like an agitation issue to me. If the bark was spent then the pulls would be getting smaller.

 

[Trickster]

Could it be because DMT partially reacts with DCM?

 

[Shaolin]

First things first
Ain't tryin' game you up so girl I'll be straight
First things first
Don't want to mess it up before it's too late
My name is... and you are?
I'd like to get to know you if it's okay

Infundibulum:
pH was checked with a pH meter (calibrated directly before the usage) and narrow range (12-14) pH papers.

In previous attempts (similar to this one, maybe some changes in the boiling time variables) I have raised the pH up to 12.9 - 13 (~20g of NaOH per 500ml of the basified solution) and there wasn't any yield increase. I'm yet to do this with the current exteaction.

For instance, once I raised it up to 13 and used hot (T= >65C) heptane (2*50ml). I got 100mg while all the previous DCM pulls gave maybe 400mg ?

end: I still have 100-200g of this batch. I will probably use it either in a drytek (limonene) or in an A/B (with naptha) just to get more data. I'll be ordering new bark, when chipped comes to town.

Noman: I don't agitate the separatory funnel, per se. I just invert it a couple of times and release the fumes. I did shook once when I used heptane pulls but the yield (look above) was still very low.

Trickster: I have only experimented with the A/B DCM. I will test with using naptha/limonene this week.

As for the reaction byproducts , I'm yet to developed an opinion since I haven't studied the research thouroughly. Thanks again end for the upload.

soulfood: The 4th pull is the largest because I left some DCM in the separatory funnel during the 1/2/3 pull and only did the dropwise technique on the last, fourth one.

Thanks everyobody. I really appreciate taking your time to help me with this issue.

 

[tele]

Might be off-topic, but maybe you can try another tek if this one doesn't yield well. I would recommend q21q21's tek.

 

[Shaolin]

Limonene experiment was conduced on the solution from the original post.

PH: ~12
Solvent: Limonene, ~130ml

Agitation was beyond furios, it took the emulsion more than a day to settle.

FASW was prepared with 1g of fumaric acid and 120ml water and filtered to remove the excess fumaric acid.

Four 30ml FASW pulls on limonene were used, each transferred to it's own petri dish.

1. pull - 110 mg
2. pull - 100 mg
3. pull - 110 mg
4. pull - 60 mg

Total: 370mg of fumarate which translates (370 * (76%) = 281.2) into 280mg of freebase.

Conclusions ? If any.