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official extraction help thread Options
 
Entropymancer
#621 Posted : 11/22/2008 7:42:23 PM

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550 is a reasonable yield (0.55%). The yellow is apt to be DMT N-oxide. It's similar in effect to DMT, and some people actually prefer this yellowish spice over the pure white. If you want to get rid of it, a simple recrystallization will do.

Hmm, can't find the pictorial tek that I'm looking for, but Entheogenist's recrystallization tek is a good one.

Also, with zinc dust, you can convert the N-oxide back to the freebase.
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
endlessness
#622 Posted : 11/22/2008 7:57:25 PM

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ploticus wrote:
swim has a question or two.

swim is doing a stb extraction on 200g of mhrb following nomans tek. The pulls were done in pairs of two mostly because swim had things to do after the first two were done and restarted this morning. The first two pulls looked promising, after checking on them last night before bed they had been in the freezer for about an hour and a half to two hours. They were very foggy white. This morning they were clearer with just a teeny tiny visible crystal floating in each of them. swim decided to evaporate half of the volume from each and try freeze precipitating again.

1) swim is thinking about combining both pulls into a single jar after they have evaporated enough, is there any reason why this shouldn't be done?

swim thinks the problem with the first two pulls was he didn't agitate well enough. it has been read that it takes a minute or two between agitations for the naphtha to completely reseparate from the soup and swim noted that it was never mixed together well enough to require a wait time for the two to seperate. swim hopes to have corrected this on the third and fourth pull.

2) swim would like to know if the above line of thought might have some merit?


1- sometimes each pull is whiter than the one that comes after. If you want to separate your spice in different colours, then dont mix the two. Some people dont care and mix it all together. SWIM usually puts the first and second pulls together, and then the 3rd,4th and 5th he puts together in another container (and usually recristalizes them afterwards)

2- sounds right. just dont agitate too strongly or emulsions will form


quilatoa wrote:
I think my friend got confused. He should have ended up with about 1000mg if he'd gotten anywhere near 1% as folks are discussing in the stickied threads on yields.

Still, he wonders, what's with all the yellow?


as for the 0,55% yield, this is normal yield dont worry. Maybe u can get a bit more by mixing the napht and letting it separate for more times before pulling it out. Also heat the naphta in warm bath and also heat the whole basidified mix in warm bath in the last two pulls. and make a fifth pull (100ml hot naphta for the 5th pull is enough, no need for 200 again).

as for the oily result.. are u sure your naphta evaps cleanly? if so, then its one of 3 things (or a mix of them) : solvent that didnt yet evap completely, a bit of plant oils that were xtracted together, or dmt n-oxide

use a knife to scrape the oil and rub it on the walls of the evapping dish again, and let it evap more. do this a couple of times. could be theres still a bit of solvent that gets trapped and does not evap, so by doing this u help it evap completely

if this still doesnt help, it can be plant oils, and the way to get rid is to put it all in a thin container, dissolve it all in a minimum amount of warm naphta (15ml in your case). in the bottom a dark layer will remain undissolved. pipette the clean naphta out and leave the goo. add 3 more ml to the goo just to make sure u got all the actives, pipete it out (the goo can be thrown out), put together with the other 15ml, and now either close the container (kitchen wrap is fine if there is no lid) and stick in the fridge overnight (will be a cleaner product) or evap again

if the yellow oil does not dry after scraping and waiting, and does not dissolve at all in the 15ml hot naphta sitting in a warm bath even after 5 mins moving it around a bit, then u got some dnt n-oxide. It is insoluble in naptha, and does not get dry. dont worry it is active. just use some herbs to soak it up, and smoke the herbs...

or make the tek elsewhere in this forum with zinc dust to turn it back into dmt


in SWIMs experience, a lot of the times when an oil doesnt crystalize in spice xtraction, it is still some solvents, and rescrapping it and rubbing on the evap dish a couple of times and waiting will usually work. lesser times are oils, and rarely it is n oxide
 
quilatoa
#623 Posted : 11/23/2008 7:43:06 AM
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My friend suspects plant oils. It's kinda sticky, even after a few hours of scraping and drying under a fan (it does seem dryer now).

Now it's now down to about 490mg (but some of that is bits of lost spice).
 
endlessness
#624 Posted : 11/23/2008 1:15:24 PM

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insist in the scraping and spreading on the evappin dish a few times more for a day, and if not, proceed to the redissolving in warm naphtha (or just scrubbing it all up with some herbs)
 
trydzyk
#625 Posted : 12/10/2008 8:35:57 AM
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I am beginning to think I got scammed. Never got anything solid from my MHRB - I tried vovin's and noman, being anal retentive when it comes to equipment and reagents (everything laboratory grade). The only thing I ever got from my attempts was sticky yellow oil, smelling like plastic + a bit mushroomy/stale smell. And there was always very little of it, even when I started using DCM, which is supposed to pull everything...

I received my MHRB pre-powdered, pinkish-brown, smelling a bit like cinnamon. Do you think my material could be shit?
 
endlessness
#626 Posted : 12/10/2008 11:33:02 AM

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well yeah if you did everything right and it still was very small yield, it can always be a problem with the starting material... its always better to buy from trustable sources
 
Infundibulum
#627 Posted : 12/10/2008 1:23:55 PM

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SWIM's FOAF never had much luck with pre-powdered MHRB. Vendors could be actually selling anything that looks like some "pinkish purple dust".

SWIM's FOAF doesn't even buy those marketing descriptions that vendors usually attach to their powdered product, i.e. that it is the real inner root part that has the highest amount of goodies or similar.

But on the other hand, for every person hating the pre-powdered stuff there is a person loving it.

Getting whole strips has never disappointed SWIM's FOAF. At least one can actually see what he/she is getting. Powdering the stuff is not a big hassle either.

On a sidenote: when powdering the root bark one gets the purple dust thing and fibres that won't really turn into powder. Once some accidental girl I chattet while waiting for the bus claimed that she separated the pink dust from the fibres and extracted them separately. She said that the fibres gave a much much bigger yield per weight than the purple pink dust.

Go figure...

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
meanderer
#628 Posted : 12/18/2008 12:14:56 AM
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SWIM was thinking about a hypothetical extraction of the dried leaves of a plant. He thinks liquid/liquid interfaces are messy stuff. So, he was wondering why wouldn't one be able to defat the dried material before extraction? In theory, all the alkaloids of interest should be in the organic insoluble salt form. And to get around the liquid/liquid interface, one could basify like a Yopo snuff, making a paste with basic solution, then extract with more solvent. Does anyone know someone who has tried this?

SWIM was thinking he could first defat the pulverized raw material with chloroform, alongside a naptha wash (until solvent stays clear). (Would this take too much solvent if working with sub-kg masses of raw material?)

Next, SWIM was thinking about making a alkaline paste out of the defatted (and dry) raw material and a minimal volume of water pH 11, then spreading it out on a dish to dry.

Once dry, SWIM was thinking about first extracting the resulting material with hot naptha, then chloroform, and evaporate each extraction separately.

It seems always filtering would be a pain in the arse, but if one were to have access to a centrifuge, life would be slightly easier.

Any thoughts?
 
meanderer
#629 Posted : 12/19/2008 12:08:32 AM
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Nevermind. SWIM found discussion on this tek here.
 
xdream
#630 Posted : 12/28/2008 9:31:46 PM

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do you not heat/cooking mix using noman tek?
Divine Moments of Truth
 
ploticus
#631 Posted : 1/4/2009 4:01:49 PM
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xdream wrote:
do you not heat/cooking mix using noman tek?

nope.


Anyone ever had their freeze precip jars look like they really really want to drop crystals. all foggy and stuff but 10 hours later after being in the freezer they are still foggy and have barely any, if any, crystals floating/stuck to the sides?

What do you guys suggest to do in this situation. I know evaping off the naphtha about 1/2 way should help but I want to save that for last as I don't want to sit around for a week or more with naphtha evaporating away in the window stinkin up the room.
 
endlessness
#632 Posted : 1/4/2009 7:39:48 PM

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ploticus wrote:
xdream wrote:
do you not heat/cooking mix using noman tek?

nope.


Anyone ever had their freeze precip jars look like they really really want to drop crystals. all foggy and stuff but 10 hours later after being in the freezer they are still foggy and have barely any, if any, crystals floating/stuck to the sides?

What do you guys suggest to do in this situation. I know evaping off the naphtha about 1/2 way should help but I want to save that for last as I don't want to sit around for a week or more with naphtha evaporating away in the window stinkin up the room.


well you dont got much choice there.. The two physical ways to make it crash out is either evaporating more (saturating) or lowering the temperature, and I guess you are already in the coldest setting of your freezer.

Just use a fan to blow the smell out.
 
ploticus
#633 Posted : 1/5/2009 2:46:35 AM
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Any estimation how long it'll take with a fan? Say 500ml or so.
 
psychonaut
#634 Posted : 1/6/2009 9:51:09 PM
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Roughly 110g mimosa was broken up as finely as possible and added to 470ml water that had been basified with 50g lye. 100ml naphtha was added and and the contents on the jar shook.
SWIM repeated the naphtha pulls the same way 3 times(soak times 15 min, 12hrs, 24hrs) and he has VERY little to show for it. the 1st 2 were evaped and the combined scrapings were maybe 20mg. The 3rd was evaped to 1/2 in in a shot glass and freeze perciped(small amount of crystals but more than the last 2 combined, and completely white. They cover the bottom of the shot glass, very thin layer) Total is probably 50mg, he has one last pull sitting in there, hopefully that gets something(he might need to try a xylene pull to get anything that is left).
SWIM was wondering, is this a problem with my technique or my starting material(also posted in suppliers for they have a bit of a sketchy reputation). If that is the case, he is going to order some more bark soon from a well trusted source. He still have 110g that he did not add to the operation in case there was a flaw in it.
So, opinions?
 
Exarp
#635 Posted : 1/10/2009 12:12:56 PM

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SWIM have question about preparing acid solution with correct pH. SWIM don't have pH meter and papers. Why? He lives in stupid country.
Now:

1. SWIM have 9% HCl, and want to use it for extraction. SWIM have read that adding 10 ml of 30% HCl to 1 l of water shoul prepare acid solution with pH 2. How to calculate how much of each to mix? Is there any formula to calculate it?
Wold it be the same if I put 30 ml of 9% HCl in 1 l of water?

2. SWIM have found n-heptane (very cheap, 1l = 4 EUR. Is it OK to use this heptane for defatting and for Spice extraction?
Just keep the balance...the middle path...
93 93/93
 
xdream
#636 Posted : 1/11/2009 3:12:12 AM

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SWIM gets sticky like oil in the pyrex that doesnt dry out from freeze metod is this commmon? Its clear not yellow.
Divine Moments of Truth
 
Infundibulum
#637 Posted : 1/11/2009 4:38:06 AM

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Exarp wrote:
SWIM have question about preparing acid solution with correct pH. SWIM don't have pH meter and papers. Why? He lives in stupid country.
Now:

1. SWIM have 9% HCl, and want to use it for extraction. SWIM have read that adding 10 ml of 30% HCl to 1 l of water shoul prepare acid solution with pH 2. How to calculate how much of each to mix? Is there any formula to calculate it?
Wold it be the same if I put 30 ml of 9% HCl in 1 l of water?

2. SWIM have found n-heptane (very cheap, 1l = 4 EUR. Is it OK to use this heptane for defatting and for Spice extraction?

Hi Exarp,

10ml of 30% HCl in 1 litre of water is utterly massive amount of acid! It will actually give SWIY a pH of 1.107. And 30ml of 9% in 1 l of water will give SWIY a pH of 1.14.

Both pHs are very high. Ideally a pH of 4-5 is more than enough. And SWIY makes it by adding just a few drops (4-5 drops) of the concentrated HCl in 1 litre of water.

An accurate pH is not very critical. And it is difficult to make a correct pH when extracting. The acids of the plant material will lower the predicted value. And when it comes to HCl, it can be boiled off the solution so when the decoction is prepared, it will be getting gradually towards more basic.

Of course all this is nonsense. Few drops of HCl is enough. And SWIY should not worry about the pH meter. If he really wants some pH indicator he can make pH papers from red cabbage. But do not be too anal about pHWink

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Infundibulum
#638 Posted : 1/11/2009 4:39:26 AM

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xdream wrote:
SWIM gets sticky like oil in the pyrex that doesnt dry out from freeze metod is this commmon? Its clear not yellow.

What is the ambient temperature in SWIY's "lab"?

Need to calculate between salts and freebases? Click here!
Need to calculate freebase or salt percentage at a given pH? Click here!

 
Exarp
#639 Posted : 1/11/2009 11:05:49 AM

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Thanks Infundibulum...you just solve my No1 problem Smile
Just keep the balance...the middle path...
93 93/93
 
xdream
#640 Posted : 1/11/2009 12:46:05 PM

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Infundibulum wrote:
xdream wrote:
SWIM gets sticky like oil in the pyrex that doesnt dry out from freeze metod is this commmon? Its clear not yellow.

What is the ambient temperature in SWIY's "lab"?


Dunno around 20c
Divine Moments of Truth
 
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