Let's calm it down please.
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Toshido's A/B Hot Plate TEK (Pictorial)
OrangeEnergy said:
It clearly states what my process borrows from, complete with hyperlinks and member credits. And again, no picture of my face.
Toshido said:
Moving on. Anyways, updates to come soon.
^This information should allow you to extrapolate a sensible value. A few minutes should suffice. Maybe ten minutes for mixing with the naphtha, but even that's a fairly generous amount.
We're looking at a partition equlibration of a non-polar solute between a polar and a non-polar solvent, at least in the latter case. Stirring brings the two phases into thorough contact fairly promptly, so it doesn't need to go on for a particularly long time.
Memberberries
Membah?
Hey Animaus, it sounds like you don't really understand the concepts at play here.
Check out Entropymancer's DMT Extraction Overview.
It's a really handy resource that will help with all of the questions you've been asking by outlining and explaining the conceptual underpinnings of the extraction process.
A little bit of reading goes a long way, and I think you'll be surprised by how many questions you'll be able to answer once you've read it
@Toshido hasn't been around for some while, but my observation is that this method is focussed on speed and purity though the use of magnetic stirring, whereas @cyb's doesn't specifically use it. The 5 repeats of manual stirring/shaking would likely achieve a similar level of contact between the aqueous and the non polar phases as a single rapid mechanical stir would.
The recommendation on background reading is also a sound one
The recommendation on background reading is also a sound one
Ethanolstalgia
Esteemed member
Toshido here! Having a hard time recovering my old account, but cool that someone dug this up and followed the TEK! I'll be continuing my extraction runs and tweaking more variables to see if I can pull more out of the bark yield wise!
Ethanolstalgia
Esteemed member
Hey Void pleasure to see you again. Thank you for helping.
First of all, thank you @Toshido for all the work you've put into making this guide so easily understandable with all the photos and documentation.
However, my friend has followed the guide to the point twice, and somehow both times something failed, as she didn't get any crystals forming in the naphtha after the freeze precipitation process (i was her first A/B extractions, after doing many successful STB extractions with the same powdered bark).
So, now she's trying to pinpoint where it went wrong. She has a few questions..
* At step 1-2 (mixing water, vinegar and MHRB for 45mins), she didn't keep a constant temperature of 70c, since the magnetic stirrer she doesn't supply enough heat to keep the temperature. So a heat bath was used to heat up the mixture to 75-80c, and while stirring it would slowly drop to 65c, then heating again to 75-80c etc etc until 45-60mins of mixing had been reached. Seems unlikely that this would affect the result, but she thought better to mention it anyway..
* At step 6 (adding 50ml of naphtha, stirring 1min, resting 1min, then pulling the naphtha), at what temperature is the mixture? And the naphtha when added to the mixture, is it at room temperature? During the pulling phase, do you take care to keep a warm temperature throughout?
During the second extraction, she did the extraction with 40ml and subsequently 30ml naphtha instead of 50ml, hoping it'd be more saturated, but without any change in result. She also kept the mixture of naphtha stirring for 5mins instead of 1min, hoping that this would make a difference, but still no crystals formed during freeze precip.
She would also like to mention...
* ...that while pouring the base into the acidic solution (step 5), she believes she saw the "DMT crash". She saw big white clouds form in the acidic solution when the base was added, which after some seconds start disappearing into the dark basified part of the solution, before the whole solution starts turning dark as night. So, she thinks that this is a sign that the acidification process was successful, and the filtered acidic solution did contain DMT as it should?
She really hopes someone is around to shed some light on this, it's very frustrating to end up with failed results after several ambitious but failed attempts!
However, my friend has followed the guide to the point twice, and somehow both times something failed, as she didn't get any crystals forming in the naphtha after the freeze precipitation process (i was her first A/B extractions, after doing many successful STB extractions with the same powdered bark).
So, now she's trying to pinpoint where it went wrong. She has a few questions..
* At step 1-2 (mixing water, vinegar and MHRB for 45mins), she didn't keep a constant temperature of 70c, since the magnetic stirrer she doesn't supply enough heat to keep the temperature. So a heat bath was used to heat up the mixture to 75-80c, and while stirring it would slowly drop to 65c, then heating again to 75-80c etc etc until 45-60mins of mixing had been reached. Seems unlikely that this would affect the result, but she thought better to mention it anyway..
* At step 6 (adding 50ml of naphtha, stirring 1min, resting 1min, then pulling the naphtha), at what temperature is the mixture? And the naphtha when added to the mixture, is it at room temperature? During the pulling phase, do you take care to keep a warm temperature throughout?
During the second extraction, she did the extraction with 40ml and subsequently 30ml naphtha instead of 50ml, hoping it'd be more saturated, but without any change in result. She also kept the mixture of naphtha stirring for 5mins instead of 1min, hoping that this would make a difference, but still no crystals formed during freeze precip.
She would also like to mention...
* ...that while pouring the base into the acidic solution (step 5), she believes she saw the "DMT crash". She saw big white clouds form in the acidic solution when the base was added, which after some seconds start disappearing into the dark basified part of the solution, before the whole solution starts turning dark as night. So, she thinks that this is a sign that the acidification process was successful, and the filtered acidic solution did contain DMT as it should?
She really hopes someone is around to shed some light on this, it's very frustrating to end up with failed results after several ambitious but failed attempts!
Hi, welcome to your first post! 
To address your questions in order:
The clouding observed on addition of base may or may not have been DMT. The bark brew contains a large number of other substances, of course - any to many of which could also contribute to the turbidity.
It does seem as though the core points of the extraction were followed correctly. There are several possible reasons for null results with freeze precipitation:
Hope this helps! Feel free to ask for further clarification.
To address your questions in order:
- The temperature fluctations during the acidic brewing phase should be of little consequence.
- Regarding solvent temperature:
- This seems to imply you'll be pulling from a hot solution, but the exact temperature varies with personal preference as well as with the exact properties of your particular batch of solvent. Somewhere between room temperature and 70°C should get you satisfactory products. Lower temperatures typically produce whiter spice, however.
- Adding naphtha to warm 'soup' rapidly equlibrates in the direction of the aqueous phase, since the specific heat capacity of water is significantly higher than that of naphtha. Similarly, cold soup would rapidly cool down hot naphtha.
The clouding observed on addition of base may or may not have been DMT. The bark brew contains a large number of other substances, of course - any to many of which could also contribute to the turbidity.
It does seem as though the core points of the extraction were followed correctly. There are several possible reasons for null results with freeze precipitation:
- weak or bunk bark
- insufficient saturation of the naphtha (too much used → evaporate or use mini A/B to concentrate)
- unsuitable naphtha composition (excessive aromatic content inhibits freeze precip →use an alternative recovery method)
- freezer not cold enough
- insufficient wait time
- new dish lacks nucleation points (→scratch it gently a few times with a fork)
Hope this helps! Feel free to ask for further clarification.
Hi, welcome to your first post!
To address your questions in order:
- The temperature fluctations during the acidic brewing phase should be of little consequence.
- Regarding solvent temperature:
- This seems to imply you'll be pulling from a hot solution, but the exact temperature varies with personal preference as well as with the exact properties of your particular batch of solvent. Somewhere between room temperature and 70°C should get you satisfactory products. Lower temperatures typically produce whiter spice, however.
- Adding naphtha to warm 'soup' rapidly equlibrates in the direction of the aqueous phase, since the specific heat capacity of water is significantly higher than that of naphtha. Similarly, cold soup would rapidly cool down hot naphtha.
Thank you for the warm welcome
And the elaborate answer. Very helpful.So, she did another extraction with several modifications, and it was successful. However, since she didn't change only one variable, but several, this reply might be not very clarifying. For this extraction, the following was done differently:
- Boiled the root for half hour, instead of trying to keep a constant lower temperature.
- Added more base, to be sure the solution would be basic enough.
- Used smaller amounts of NPS for extractions - around 30ml/pull to achieve higher saturation.
- Performed all extractions at ˜60-75C for 30mins stirring at 1200RPM.
I've never boiled my acidic solution or my basic solution so that may be too hot. As far as adding base, the rule is 1:1 so 50g MHRB to 50g NaOH, 50mL is what you should be aiming for when pulling solvent, it doesn't matter if the solvent is saturated, it just takes longer for it to evaporate if you want to fast evap before freeze precipitation, and 1200RPM is a bit too high for mixing, you're at the thresh hold and gonna get emulsions that way, which makes pulling a lot harder. Hope this helps.Thank you for the warm welcome
So, she did another extraction with several modifications, and it was successful. However, since she didn't change only one variable, but several, this reply might be not very clarifying. For this extraction, the following was done differently:
This produced a decent result, with about 0.7% pulled in the first three pulls. Later more pulls were performed, with good results, but they haven't been weighed yet.
- Boiled the root for half hour, instead of trying to keep a constant lower temperature.
- Added more base, to be sure the solution would be basic enough.
- Used smaller amounts of NPS for extractions - around 30ml/pull to achieve higher saturation.
- Performed all extractions at ˜60-75C for 30mins stirring at 1200RPM.
