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Things I have learnt about Confusa and Rue Extractions.. Options
 
confucius
#1 Posted : 2/23/2014 2:57:01 AM
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Howdy Folks - my first post here. Been lurking for a couple months and have observed SWIM doing extractions on rue and confusa. Swim is a scientist by training, altough more on the biological / statistical side of science than hard Organic Chemistry like other folks here.

Things I've learnt from SWIM's trial and error:-

Rue

Control A (crushed seeds) vs Treatment A (non-crushed seeds) - no difference whatsoever in Harmala extraction quantities - conclusion - crushing the seeds is a PITA and not really worth it.
Control B (multiple boils whole seeds) vs Treatment B (Three day soak in 1M HCL solution just covering 400G seeds) - Treatment B has 95% yield vs Control B (20g Harmine, 17g Harmaline after multiple washes) - conclusion - it's not worth the trouble of boiling and combining the boils - one long soak suffices..

Acacia Confusa A/B

ACRB is very oily and you should do at least one acid phase defat using naptha if you want to reduce the quantity of these oils coming through to the final product.
Heating during acid phase is worthwhile, but heating or warming the base phase to increase the pulling power of your solvent, whilst effective, also seems to pull remnant plant fats. Before SWIM learnt this, he had many pulls which included honey coloured liquid (often called jungle spice) from ACRB. This liquid would dissolve all spice shortly after evap or precip using FASA. SWIM doesn't think this is NN DMT, NMT, DMT-N-Oxide or that Jungle Spice is anything real - he believes it's plant fats that are very effective at dissolving Spice - hence the reason that the MS analysis of this substance shows high quantities of alkaloids.
Using NO HEAT during base phase pulls reduces or eliminates this contamination.
To support this contention, SWIM Generally does 4 Naptha Pulls (Cold), then 2 Xylene Pulls (Cold) - the xylene to clean up any full spectrum remnants. If either the Napptha or the xylene is warmed, he gets the 'jungle spice', if done cool, no 'jungle spice' - even though yields are high relative to 'normal' - The Naptha Pulls yield around 1/3 of the Spice, the Xylene pulls yield 2/3. Swim precips using FASA and keeps the Naptha and Xylene pulls separate. ZERO 'Jungle' - just white crystals, total ~ 1.6%

SWIM is currently gearing up for his first oral biossay - 70mg Harmine Freebase, 60mg THH Freebase (produced using Zn+HCL Redox with High PH NaOH precip), 6.5mg Harmaline freebase, 60mg DMT Fumarate and 500mg Ascorbic acid to salt the freebases for better absorption and neutralise any remnant Lye, Na2CO3 or NAHCO3- all mixed in 70ml of H20. Plans to take two of these doses 1 half hour after the other. It's taken two months of preparation and lab work to get to this stage, so Swim feels a sense of trepidation. Will report.

Have fun..

(Mods I munted this up and placed in FAQ section instead of introductory essay - could you please move for me? Ta)
 

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confucius
#2 Posted : 2/23/2014 4:29:10 AM
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Ah.. by the way - a tangent. I've seen the smoked dmt 'carrier wave' described in another topic in which I cannot post.. for my friend it sounds just like the bullroarer depicted at 1.40 in the following croc dundee clip - Crocodile Dundee Bull Roarer
 
Earthwalker
#3 Posted : 2/23/2014 7:39:12 AM

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Hi Confusius , and welcome
Are you saying you should have ( cool base soup and cold naphtha pulls ) or just ( cold naphtha pulls ) into normal basified soup ! So not to pull the oils and other impurities Mainly resulting in goo and melting not fully formed crystals ??
 
boogerz
#4 Posted : 2/23/2014 8:46:15 AM

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Welcome Confucius!

Thanks for the intro & sharing your results. I've also had similar results from working with rue and will never grind them up again.

Hope you stick around and see you around.

 
confucius
#5 Posted : 2/23/2014 8:59:58 AM
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Hi Earthwalker - Fellow Aussie, I suspect!

When I say 'cold' I actually mean room temperature.. so basically defat your hot acid soup, let it cool to room temp and your pulls (whether Xylene, DCM, Toluene (YUCK!), Limonene - name your solvent) - don't warm them. Keep them at room temperature also.

Many of the Mimosa techs call for warming the base soup - or prewarming the solvent to enhance the pulling power of the solvent. Not necessary, imho, at all - but with ACRB, not advisable full stop - too much fat in the soup. My theory is that these oils are relatively insoluble at room temp - if you don't heat the soup, you leave the oils behind.

For those really keen to explore the jungle, then, by all means, do a final 'hot soup pull' after the 3 x naptha 2 x Xylene pulls and bioassay.. there'll be plenty of 'jungle' to play with.. best for making acacia soap.

All the best - C
 
confucius
#6 Posted : 2/23/2014 9:09:46 AM
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Hi Boogerz!

Thanks for the thanks and sentiments Smile

At this stage Swim's probably got enough spice to last until the next millenium so maybe after this upcoming oral bioassay (tomorrow is the date, fyi), visits for insight may be less regular, but time will tell!

C
 
Earthwalker
#7 Posted : 2/23/2014 9:47:24 AM

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confucius wrote:
Hi Earthwalker - Fellow Aussie, I suspect!

When I say 'cold' I actually mean room temperature.. so basically defat your hot acid soup, let it cool to room temp and your pulls (whether Xylene, DCM, Toluene (YUCK!), Limonene - name your solvent) - don't warm them. Keep them at room temperature also.

Many of the Mimosa techs call for warming the base soup - or prewarming the solvent to enhance the pulling power of the solvent. Not necessary, imho, at all - but with ACRB, not advisable full stop - too much fat in the soup. My theory is that these oils are relatively insoluble at room temp - if you don't heat the soup, you leave the oils behind.

For those really keen to explore the jungle, then, by all means, do a final 'hot soup pull' after the 3 x naptha 2 x Xylene pulls and bioassay.. there'll be plenty of 'jungle' to play with.. best for making acacia soap.

All the best - C


Yes mate and a proud Aussie at that !!

I'll try the cool pulls on a small amount and see how I go , thank for the info , I look forward to reading you're future posts and contribute's to the nexus !!Thumbs up
 
confucius
#8 Posted : 2/23/2014 10:23:25 AM
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Thanks Earthwalker -

I'm sure you know, but, tip for other Aussies.. all our Naptha (shellite) has crud in it. If you do a full evap of a Shellite pull and smoke the base, you're going to cough your guts out and feel like your lungs want to jump out of your chest and go directly to ER.. I've used a few Napthas here but Diggers is prob the least crappy, but still crappy.

IMHO in Aus if you're planning to imbibe by breathing, nothing beats ACRB->HCL->NaOH->Shellite->Cold Precip->Decant and turn it upside down in the freezer to let all Shellite run away -> Dissolve in Acetone-> Precip in FASA-> Filter through Filter Paper and let air dry with paper still in funnel -> Pour a great big dollop of Acetone through the filtrate -> Freebase in Na2CO3 -> Dry -> Imbibe. This way you wash every last bit of that Shellite crud away and reduce your hydrocarbon impurities.

Freebasing from Cold Precip Naptha, Atmospheric Evap and Imbibe as our US friends do is the height of madness here, particularly given the high benzene (= major carcinogen) content of our Naptha compared to other countries..

Happy travels!

 
DreaMTripper
#9 Posted : 2/23/2014 11:08:01 AM

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Welcome to the nexus many thanks for your helpful experiments! Im curious as to where you sourced fumaric acid from in Aus youre the first Aussie to mention using it.
For reX many have had good results using undu heptane and sceneys shellite has also been touted as a reasonable naptha..
It sounds like you would have good opinions to contribute to this thread https://www.dmt-nexus.me...aspx?g=posts&t=41776
 
confucius
#10 Posted : 2/23/2014 11:15:40 AM
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Hi DreaMTripper -

I obtained my Fumaric Acid from overseas.. indeed it's about impossible to get here directly but totally necessary to have imho. If anyone would like some for ethnobotanical research purposes only, they're welcome to PM me.

+ thanks for the tips!

C
 
SnozzleBerry
#11 Posted : 2/23/2014 3:01:02 PM

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Just to point out, with regards to the acid phase, you can skip the defats, which can be time consuming/wasteful.

Instead of defatting, you can back-salt your end product out. So, do your acid soaks, basify, pull with your solvent (something along the lines of xylene, toluene, dcm, d-limonene...not naphtha or similar) and then salt your DMT out of solvent using FASW, vinegar, or another acidified solution. This leaves you with with DMT fumarate, DMT acetate, or another salt form, depending on the acid used. Then you can do a water conversion back to fb if you used FASW, or a mini a/b if you used vinegar.

Just an option for avoiding defats Smile

Also, I've found drastically different results when it comes to rue extraction, regarding the differences between ground/whole and performing multiple rounds of pressure cooking vs a single soak or boil. I know results for ground seeds have gone back and forth...so this comment isn't meant to invalidate your results, but rather to highlight that there does seem to be varied results when it comes to these comparisons and that people may wish to experiment for themselves and see what they find.

Thanks for sharing your info and results with us Smile

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Jees
#12 Posted : 2/23/2014 9:57:50 PM

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Rue:
confucius wrote:
...Three day soak in 1M HCL solution just covering 400G seeds...one long soak suffices...

1 week cold soak of whole seeds in 0.02 M HCL (pH 1.7), daily shake, and almost no result, needed boiling to get results. Seems your concentration of 1 M (pH 0) did the trick on the whole seeds in cold water.

With ground seeds this 0.02 M cold soak worked like a charm, not for the whole seeds.
 
confucius
#13 Posted : 2/24/2014 4:06:15 AM
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Snozzleberry - ta for the advice FASW is not a method SWIM's tried just yet, but your method is novel and he will explore. I guess a reason Swim does an Acid defat (only 1 - he lets it go while the ACRB is steeping after boiling - and reuses the shellite) is that he figures since the salts aren't soluble in Non Polar Solvents, there is no loss, and the removal of the oils and fats means the goodies in the NPS base phase aren't competing with fats to be dissolved.

Jees - ta for the feedback - I'd be interested to see what happens if you try with the stronger acid - report back Pleased

BTW - there was some discussion on the boards some while back about potentially using electrolysis for reduction of Harmaline to Tetrahydroharmine, rather than using the Zinc dust method - does anyone know if that's gone any further?
 
dmt_spider
#14 Posted : 2/24/2014 9:12:02 AM

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confucius wrote:
I'm sure you know, but, tip for other Aussies.. all our Naptha (shellite) has crud in it. If you do a full evap of a Shellite pull and smoke the base, you're going to cough your guts out and feel like your lungs want to jump out of your chest and go directly to ER.. I've used a few Napthas here but Diggers is prob the least crappy, but still crappy.


Which brands did you test? How did you test them to come to these conclusions?

Also, how far south are you? South across the strait South?


 
dmt_spider
#15 Posted : 2/24/2014 11:03:30 AM

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Further to the above, when looking at the MSDS for various Australian brands of shellite I see:

KCB Shellite (available in S****cheap)= ethylbenzene is listed last in the components that make up this shellite, but it doesn't say what quantity as a %

Diggers Shellite = <0.1% w/w benzene, same as Zippo and Swan

Sceneys Shellite = it lists n-Hexane and toluene but no benzene is listed at all.

Hateleys Shellite = lists a few compounds but benzene is not one of them, although it does list "other hydrocarbons" at the bottom of the list so it may be in there.



 
confucius
#16 Posted : 2/24/2014 9:43:59 PM
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Hi DMT_Spider - He tried KCB and Diggers - they're the only ones available to him at his location which is around 27 degrees South of the equator Pleased

Both left a pong and oily residue which didn't give a huge amount of confidence - and he also read the MSDS on both which pointed out the benzene content. Benzene in any amount is not something he wants to imbibe or be exposed to if at all possible.
 
confucius
#17 Posted : 2/24/2014 10:08:05 PM
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Quote:
SWIM is currently gearing up for his first oral biossay - 70mg Harmine Freebase, 60mg THH Freebase (produced using Zn+HCL Redox with High PH NaOH precip), 6.5mg Harmaline freebase, 60mg DMT Fumarate and 500mg Ascorbic acid to salt the freebases for better absorption and neutralise any remnant Lye, Na2CO3 or NAHCO3- all mixed in 70ml of H20. Plans to take two of these doses 1 half hour after the other. It's taken two months of preparation and lab work to get to this stage, so Swim feels a sense of trepidation. Will report.


By the way - Swim kept to his word and he and a friend partook in the pharma brew mentioned above.

Swim's friend is around 70kg, and he's around 90kg, so they modified the doses slightly..

Little guy - 45mg DMT Fumarate:45mg THH:55mg Harmine:5mg Harmaline
Big guy - 55mg DMT Fumarate:55mg THH:67mg Harmine:6mg Harmaline

1 gram ascorbic acid was added to each dose, and around 70ml water. Mixture was shaken and allowed to stand for a couple hours.

First dose was taken at 5.45pm, second around 6.20pm. Effects came on strongly ~7.20pm, so pretty much bang on 1 hour after the second dose. Main effects were largely complete by 22.00 - although it seemed like a heck of a lot longer.

So the experience took ~1.5 hours to commence - came on very strong after a piece of bread eaten. The little guy had a very strong purge as the effects commenced - with obsessively purified harmalas - so I guess the purge is just part of the experience for some folks - pharma or non-pharma.

The big guy had extremely vigorous rhythmic 'convulsions' accompanying the peak of the psychedelia - I guess is a way to describe it - involuntary strong leg and hip movements that felt like part of 'the work'.. and seemed to 'beat with the rhythm of the experience'. Occasionally they'd pause for a while and he'd feel worried his heart had stopped - but that was something symbolic only and his heart was just fine.. and it'd begin again. Looking at it from a medical perspective - could this have been a 'seizure' due to SEROTONIN SYNDROME? Not sure whether it's 'just part of the experience' or worth considering further. Advice anyone?

Suspect first dose was relatively ineffective - will try separating harmalas next time and using the spice @ T+15 minutes instead.

nonetheless, It was a very powerful experience. Swim thinks dose was just about spot on for first pharma journey, although subjectively it seemed that big's experience was a fair bit more intense (although still very full) than little's experience so perhaps there was just way too high qty of harmalas overall, little was able to purge it, big had to cop it... Swim says he may just try one dose instead of two next time, segregate the harmalas from the spice and be a little more patient before downing the second brew.
 
dmt_spider
#18 Posted : 2/25/2014 2:20:04 AM

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confucius wrote:
Hi DMT_Spider - He tried KCB and Diggers - they're the only ones available to him at his location which is around 27 degrees South of the equator Pleased

Both left a pong and oily residue which didn't give a huge amount of confidence - and he also read the MSDS on both which pointed out the benzene content. Benzene in any amount is not something he wants to imbibe or be exposed to if at all possible.


You made the statement earlier:

Quote:
Freebasing from Cold Precip Naptha, Atmospheric Evap and Imbibe as our US friends do is the height of madness here, particularly given the high benzene (= major carcinogen) content of our Naptha compared to other countries..


I think this is inaccurate and could cause unnecessary worry to those of us in Aus who take our health seriously. There are two reasons why:

1) As I pointed out earlier, the MSDS for many of the shellites (aka naphtha) in Australia either list no benzene as a component at all, or in the same small amounts as that found in the US (eg: <.1% for Australian Diggers which is the same as US Zippo)

2) Research shows me that benzene evaporates very quickly into the air. Therefore if one is doing a cold precip followed by at least 20 minutes (or 45 minutes if you are particular like me) in front of a fan to get rid of any trace of naphtha smell as per the teks on this site, there should be no shellite/naphtha and therefore no benzene left in the final product. I am no chemical scientist though so I could be wrong.
 
Earthwalker
#19 Posted : 2/25/2014 3:10:58 AM

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Hi dmt_spider !Thumbs up
In you're Experiance what solvent have you found best to suit the art of extracting in OZ ??Smile
 
dmt_spider
#20 Posted : 2/25/2014 3:49:01 AM

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To be honest I'm still experimenting. I have used mainly Diggers and that has worked great. I used Zippo premium which was much more expensive and didn't seem to do any better than Diggers, in fact it seemed to pull more bright yellow plant fats.

Haven't tried KCB, it's on my list to try down the track, and I have a bottle of Hateleys but haven't tried that either. On one extraction recently I used Sceneys after I did a couple of pulls with Diggers and it seemed to pull very well indeed, so I am interested in using it straight up and seeing the difference between that and Diggers. I think the reason it pulled nicely was because it has a small amount of toluene in it which the Diggers does not.

 
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