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Large Naphtha loss in pull Options
 
TrippyLich
#1 Posted : 8/12/2019 6:06:43 PM

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I'm attempting Cyb's A/B salt tek, but seem to be running into trouble. I have very large naphtha losses between adding to the basified solution and pulling to a glass dish and also received a zero pull Sad. I'm wondering if someone with experience could help me troubleshoot where I went wrong, or what I should do to fix my extraction. My process was:

- Blend 100g Acacia Acuminata Typical Phyllode (AATP)
- Add 400mL demineralised water heat at 50°C for 1hr. Then freeze/defrost x3
- Add 100mL water and some white vinegar. Add vinegar until pH 3 result on Universal Indicator Paper
- Apply Heat at 50°C for 10 hours cool and sit 24 hours.
- Add 50mL naphtha, agitate and settle, pull naphtha, discard (Defat)

- Add 1L saline solution containing 75g deionised NaCl
- Add 200mL water with 60g NaOH for pH 13.5, rest for 24 hours agitating occasionally

100mL Diggers shellite (Naphtha/NPS) was agitated/settled repeatedly over a day or two, room temperature was 8°C to 16°C. When pulled there was only approx. 30mL left. I tried evaporating until a white cloud would form, but used a large fan and accidentally over evaporated to about 5mL. I re-saturated with about 15mL shellite and freeze precipitated for zero yield.

I moved the soup to 3 more manageable jars and tried adding about 100mL total for all. Agitated and pulled over 45 minutes, freeze percip for again zero yield.... However, My bark and 200mL soup was left in the primary container so I moved all that to a 1L container and added about 750mL more basified soup.
- Add Diggers Shellite from failed pull (This was 75mL)
- Agitate occasionally over 2 days
- Pulled only 35mL Naphtha that doesn't cloud when blown on.

I'm feeling very discouraged right now and don't know what to do. I have another 100g of narrow Phyllode. I roughly repeated the same process with no heat or defat, then heated 200mL naphtha and added to the solution. After almost 2 hours almost no naphtha has resolved to the top of the soup.

I can all but guarantee the bark is fine, so the only problems I can think of are:
- Diggers Shellite is a poor NPS
- Human error somewhere along the way

Could someone please advise where I could have went wrong, and what I could do to fix this if possible? I've taken photos of every step, so I can send anything if needed.
 

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TrippyLich
#2 Posted : 8/12/2019 6:17:39 PM

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I just seen someone with a similar issue and saw low base cited as a common mistake for newbies. I used universal indicator paper, but it just hit me I'm colour blind and may have misread the indication. Are these about 13?
TrippyLich attached the following image(s):
pH_Help.pn.png (10,127kb) downloaded 91 time(s).
 
downwardsfromzero
#3 Posted : 8/17/2019 10:50:53 PM

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pH colour looks fine. It's likely that the phyllodes [materials] were simply inactive. But then you say you were using bark? Why use bark when the phyllodes themselves would be active?




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
leratiomyces
#4 Posted : 8/18/2019 4:29:13 AM
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Hi trippy

I've never done cyb's tek, but have forged my own way with acacia phyllodes.
Some suggestions;
An aqueous solution of 1.7L is difficult to extract with 100ml of solvent. Not impossible, but difficult. You would need to shake vigorously for an extended period. The catch 22 being the longer you shake for and the more vigorously you shake, the greater the chance you form an emulsion. Emulsion risk is also increased by leaving the plant material in the mix during extraction, which you have done.
You have formed an emulsion, hence your poor recovery of shellite after you shake and allow to settle. But I suspect that this is not the only thing that has gone wrong for you, as you said you got nothing from the shellite that did separate.

Why not use a method that has been used most consistently for phyllodes.
Grind phyllodes finely.
Boil in dilute vinegar for 1h.
Filter.
Repeat two more times, filtering each time.
Combine filtrates and reduce to a workable volume.
Defat if you like.
Basify to 12 plus.
Extract with non polar several times.

Hope that helps.
 
d.b.o.
#5 Posted : 8/19/2019 6:25:41 AM
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placing the entire reaction vessel in a warm water bath and getting the entire basic solution (and lost naptha)to around 90 f layers will separate quickly regardless of the extent of mixing and shaking i subject it to. this is where thorough and effective pulls happen time frames shortened since vigorous shaking and mixing of repeated pulls 3-5 smallish well mixed pulls over a 90 min period in this heated state grabs large % of goods and most 'lost' naptha can be recovered from broke emulsion as well.
1. only use hot water bath or similar NO flames or direct heat.
2. shaking and mixing vigorous and thurough but carefully with proper saftey. I use liqor bottles for reactions very strong glass ,takes heat /cool well.literally made for holding a chemical and only plastic small FOODSAFE and chem resistant lid that occasionally contacts basic soup. mason jars are worthless imo
3. i always have reaction vessel within secondary container sink, bucket pan with hot water bath . ALWAYS only had 1 reaction vessel (liquor bottle) fail and break with over 1500ml basic soup+ 120grams root. extremely grateful my safety gear was in use and i had secondary vessel (sink) contained an otherwise serious accident
 
TrippyLich
#6 Posted : 8/19/2019 4:04:17 PM

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leratiomyces wrote:
Hi trippy

I've never done cyb's tek, but have forged my own way with acacia phyllodes.
Some suggestions;
An aqueous solution of 1.7L is difficult to extract with 100ml of solvent. Not impossible, but difficult. You would need to shake vigorously for an extended period. The catch 22 being the longer you shake for and the more vigorously you shake, the greater the chance you form an emulsion. Emulsion risk is also increased by leaving the plant material in the mix during extraction, which you have done.
You have formed an emulsion, hence your poor recovery of shellite after you shake and allow to settle. But I suspect that this is not the only thing that has gone wrong for you, as you said you got nothing from the shellite that did separate.

Why not use a method that has been used most consistently for phyllodes.
Grind phyllodes finely.
Boil in dilute vinegar for 1h.
Filter.
Repeat two more times, filtering each time.
Combine filtrates and reduce to a workable volume.
Defat if you like.
Basify to 12 plus.
Extract with non polar several times.

Hope that helps.


Thanks for the replies everyone. I’m unfamiliar with filtering phyllodes and soup (But it seems logical). My only question is, how will I know when DMT is exhausted from the bark if filtered from the solution, could you direct me to some forums on teks that do/mention this?

For my current tek: Before these replies I added Extra Lye and ~600mL saline to the narrow phyllode solution. It helped, but emulsions were still present. Based on the advice given above, I plan to do the following (Current soup photo attached, soup moved to a 3L Erlenmeyer >2L polar and 200mL NPS):
- Add more lye (lye was added 2 days before 2nd salt solution)
- Heat to 45°C (~115°C) gently stirring for 1 or 2 hours
- Pipette DMT containing Naphtha (ideally)
If failure to separate still occurs:
- Filter solution to separate phyllodes and soup
- Agitate soup again, then wait for layers to separate
- Pipette DMT containing Naphtha (ideally)

Would you (or anyone else) agree with this? I’m also curious how many mL of naphtha you use, per gram of bark, per pull in extractions for acacia phyllodes? For 1.7L being difficult for 100mL are you saying I should add more solution or naphtha? Sorry for all the questions.
TrippyLich attached the following image(s):
Emulsions.jpg (4,221kb) downloaded 46 time(s).
 
leratiomyces
#7 Posted : 8/20/2019 10:17:41 AM
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For the solution in the photo, I would allow it to sit in a hot water bath at about 60 degrees or so, and gently swirl to try to break that emulsion in the middle.
There is a stack of info on this site on how to break emulsions, everyone has their favourite technique and there are many.


The following methods are tried and tested for acacia extraction.
https://wiki.dmt-nexus.m...andbook#The_DMT_Handbook

And

https://wiki.dmt-nexus.me/Lextek

They are a decent starting point.

It's also worth reading this thread,
https://www.dmt-nexus.me...aspx?g=posts&t=35632

And finally, no, I wouldn't filter after basifying, unless I was using filtering as a means of breaking an emulsion and was convinced that the alkaloids were already dissolved in the solvent, and not floating around the aqueous solution as a solid. Filtering through celite under vacuum can break an emulsion, but most would not use this method.

Hope that makes sense.
Let us know how your narrow phyllode extraction goes.
 
 
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