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official extraction help thread Options
 
pitubo
#2001 Posted : 3/16/2014 3:21:01 PM

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dakkapel wrote:

Problem: No crystallisation after 4 times freezing and carbonate wash Crying or very sad

This week I continued. I did two pulls.


You may still try another pull, this time keeping the temperature around 35 deg.Celcius while mixing the mimosa soup and the naphta. You could do so using a warm water bath.

Quote:

After freezing I noticed transparent white slimey balls were formed in combination with a lot of brown stuff on top.


To me, the brown stuff sounds like plant remains that got shaken into your naphta. It can be removed by either recrystallization or another A/B.

Quote:

I added extra nafta heated it. Separated the brown stuff on the bottom and tried freezing again... Still brown sludge.


Good, you tried to recrystallize. Did you leave the container with the product in warm naphta standing for a little while (while still keeping the naphta at temperature)? That should allow any plant solids to fall down to the bottom, while keeping the alkaloids dissolved. When the naphta has sufficiently clarified, you can then decant the clear naphta into another container and let it cool down for crystals to form.

Quote:

So I did a Carbonate wash with two dH2O washes.
Evaporated 50%. Put it in the freezer.

Now almost 24hrs of freezing later. There are no crystals formed. Just ochre yellow fine particles on the bottom of the dish. Which are moving when you move the dish. Floating almost.


These might be goodies, in the form of really small crystals, that appear more like snow.

OR - these might be water crystals, a leftover from your dH2O washes. If so, they will melt and possibly appear slimey, but should also evaporate cleanly after decanting the (still ice-cold) naphta from the crystals. It may be helpful to use a syringe for that.

BTW, 24 hours of freezing is not excessive, sometimes it needs even longer time in the freezer to precipitate everything

Quote:

What to do? Re-X? First totally evaporate?


Try:

1. Total evaporate (get rid of any water)
2. Redissolve in minimal amount of hot naphta, let stand 10 minutes while keeping the naphta hot.
3. Decant carefully into clean container.
4. Cool and freeze for at least 24 hours.
5. Decant and evaporate last naphta remains.

Hopefully that will improve your results. If not, try A/B on it as suggested.
 

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slugware
#2002 Posted : 3/17/2014 6:35:12 PM

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hello,
i am doing an extraction right now and for the first time, just after salting a strange layer separated in the acidified and (after that) in the basified mix . This has never occured so far in my previous (six) extractions. I am applying Cyb's hybrid salt tek to the letter.

pictures 1 and 3 are few minutes after adding the salted water solution, as soon as i noticed this. picture 2 is after basifying.

is this an emulsion? i am leaving the basified solution overnight and will be pulling tomorrow, so i just wanted to check with fellow nexians what this might be.

dumb me: forgot to point out - plant material is mh
slugware attached the following image(s):
ALIM1678.JPG (2,244kb) downloaded 227 time(s).
ALIM1679.JPG (2,481kb) downloaded 226 time(s).
ALIM1677.JPG (2,108kb) downloaded 226 time(s).
 
Du57mi73
#2003 Posted : 3/18/2014 3:36:46 PM

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Looks like you had some soap in your container before using it or something to create suds.
"I am cursed by the blossoming knowledge of my feminine ideal and she looks suspiciously like you."

"Everybody is a genius. But if you judge a fish by its ability to climb a tree, it will live its whole life believing that it is stupid." -AE
 
Earthwalker
#2004 Posted : 3/18/2014 4:15:19 PM

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Du57mi73 wrote:
Looks like you had some soap in your container before using it or something to create suds.


I never use soap or detergent on my glassware , I've read many a fail just from left over residue !
 
slugware
#2005 Posted : 3/18/2014 11:12:49 PM

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Du57mi73 wrote:
Looks like you had some soap in your container before using it or something to create suds.



i did 3 pulls today, yielded approximately .6 g spice from 45 g bark.

I remember i did wash this reaction bottle like few weeks ago with a kitchenware detergent, but rinsed it with water quite thoroughly.

IF it is suds, as you suggest, it should have come frome the little pot that i use to make my acidic solution and saline solution.
Nevermind, will be more careful for that from now on.

Is there any chance that sud has affected the freebase spice. I mean reacted with it in some unknown (for me) way. Spice looks normal, at least to my understanding, but I'll be taking the extra mile re-xing and doing sodium carb washes on that yield. Just want to inquire nexians more experienced than me.

thanks for taking time to help me out.

 
decibel
#2006 Posted : 3/19/2014 10:08:57 AM

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Hi there!

I made my first extraction a month or so ago. I went for the DMT Handbook A/B extraction, and when I got to the end result I saw I had done a very sloppy work. The final product was smeared in black goo and plant oils. The siphon method, for seperating the naphta from the tea, did not work for me.
So I did a sodium carbonate wash, on which I poored 3-40ml of naptha for each gram of spice I was guessing on I had. Then I seperated the layers with 3ml syrenges, and kept te plant oils in a jar. This gave me a quite nice product Big grin

My question is now.. This jar with plant oils still contained some naphta, which after a while seperated from the other fluids.. But after the hard work of seperating with syrenges, I ordered some seperatory funnels wich I thought I would wait for before seperating the naptha from the oils.. It has now been around 3 weeks, and the jar with plant oils and naptha has been standing (very stupidly) in the sun for these 3 weeks.


Would it be safe enough to use this naptha, or should I throw it out?
And how should I approach it before hand? Should I wash it once more in Sodium Carbonate?

- It used to be seperated in to 3 layers: black, honey, naptha. Now its brown and naptha.
 
neo-kusto
#2007 Posted : 3/20/2014 10:42:53 AM
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i have used STB tek (from Watcha) and i have got from 250 gr mimosa only 0.9 gr crystals and 0.9 gr GOO
what could be wrong ? i was expecting for 4-5 gr of crystals...

pls help since i have more 250 gr mimosa

is it possible because the solvent was in the freezer only 10 hours,but its good freezer
 
neo-kusto
#2008 Posted : 3/20/2014 10:44:41 AM
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one more please..
do i need to dry the GOO? its so oily,so i dont know if it naphta or oil?
 
pitubo
#2009 Posted : 3/20/2014 1:37:51 PM

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neo-kusto wrote:
i have used STB tek (from Watcha) and i have got from 250 gr mimosa only 0.9 gr crystals and 0.9 gr GOO
what could be wrong ? i was expecting for 4-5 gr of crystals...


Don't worry too much about yields if you are new to doing extractions. Be happy that you got some already.

If you still have the basified mimosa soup, you can add some more lye, add table salt and do some more extractions with naphta. Maybe let it stand for a week or more before pulling the naphta.

Don't throw the naphta from freeze precipitating away either, it probably still contains some product. You can reuse it for more extractions or evaporate it to get the last (less pure) dmt from it.

neo-kusto wrote:
is it possible because the solvent was in the freezer only 10 hours,but its good freezer


Sometimes crystal growth just needs a little time, even in a good freezer.
 
neo-kusto
#2010 Posted : 3/21/2014 8:11:08 AM
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pitubo wrote:


If you still have the basified mimosa soup, you can add some more lye, add table salt and do some more extractions with naphta. Maybe let it stand for a week or more before pulling the naphta.

Don't throw the naphta from freeze precipitating away either, it probably still contains some product. You can reuse it for more extractions or evaporate it to get the last (less pure) dmt from it.


"

i didnt know that salt should be added,can u clarify that please, when do i add the salt,and how much ? i am using this tek

http://dc438.4shared.com/doc/hKxEpYxv/preview.html

when i mixed mimosa and lye,it was in a jar about two days..
i have used ratio 1 gr lye - 15 cc water. should i use less water?
 
cyb
#2011 Posted : 3/21/2014 8:30:43 AM

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Quote:
i didnt know that salt should be added,can u clarify that please, when do i add the salt,and how much ? i am using this tek

See HERE Wink
Please do not PM tek related questions
Reserve the right to change your mind at any given moment.
 
decibel
#2012 Posted : 3/28/2014 9:33:16 AM

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I posted this 9 days ago with no answers, so I'm trying once more (:

decibel wrote:
Hi there!

I made my first extraction a month or so ago. I went for the DMT Handbook A/B extraction, and when I got to the end result I saw I had done a very sloppy work. The final product was smeared in black goo and plant oils. The siphon method, for seperating the naphta from the tea, did not work for me.
So I did a sodium carbonate wash, on which I poored 3-40ml of naptha for each gram of spice I was guessing on I had. Then I seperated the layers with 3ml syrenges, and kept te plant oils in a jar. This gave me a quite nice product Big grin

My question is now.. This jar with plant oils still contained some naphta, which after a while seperated from the other fluids.. But after the hard work of seperating with syrenges, I ordered some seperatory funnels wich I thought I would wait for before seperating the naptha from the oils.. It has now been around 3 weeks, and the jar with plant oils and naptha has been standing (very stupidly) in the sun for these 3 weeks.


Would it be safe enough to use this naptha, or should I throw it out?
And how should I approach it before hand? Should I wash it once more in Sodium Carbonate?

- It used to be seperated in to 3 layers: black, honey, naptha. Now its brown and naptha.




Keep in mind, that the jar I mention has been standing for over a month now (:
 
pitubo
#2013 Posted : 3/28/2014 4:33:38 PM

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decibel wrote:
I posted this 9 days ago with no answers, so I'm trying once more (:

decibel wrote:

..snipped by me..


Keep in mind, that the jar I mention has been standing for over a month now (:


I read your question, and couldn't make much sense of it. Maybe you should have asked your question in a better way for people to understand and answer.

What material were you extracting anyway, that contains so much plant oils?
 
decibel
#2014 Posted : 3/29/2014 12:10:28 AM

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pitubo wrote:
I read your question, and couldn't make much sense of it. Maybe you should have asked your question in a better way for people to understand and answer.

What material were you extracting anyway, that contains so much plant oils?


Sorry for that, I did my best trying to explain my self with the english I know, but I'll try even harder!

I did a MHRB extraction, using the DMT Handbook extraction tek..
It is not that the material I were extracting contained a lot of oils, but that I wasn't thorough enough when isolating the naphta from the bark tea.
I used the siffon a siffon device like they recommended in the DMT handbook, which didn't work at all for me. I would always get lots of bark tea in the naphta container, or leave lots of naphta in the bark container.

So after washing my end product - using syrenges instead of the siphon device - I kept the oils, which I had read could be used for changa, (please correct me if this is wrong) in a jar. In this jar there was still some naphta left that first separeted after a while, which I have waited to isolate, since I have been waiting on separatory funnels to do the work Smile

My question is: Would it still be safe to use this naptha and/or plant oils after a month? If so, should I do a Sodium Carbonate wash before hand?

Hope it makes more sense this time Thumbs up
 
just-yb
#2015 Posted : 5/31/2014 7:11:58 PM

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swim got into some trouble with my last extract.
swim did and stb and usually the naphtha goes yellow.
bit this time swim became as black as the bark/base/water mix.
swim needed a light to see the layers.
and when swim friezed it the dark brown/black gue came to the bottom with nice white crystals on top.
but a soon as swim got it out of the freezer the black stuff melted as well
and swim got some really black brown crystals.
that couldn't even be recrystallized now swim discovered that when swim first cool the naphtha
it separates so swim spitted it up and friezed it again now it was nice.
and the blackish crystals swim washed with d h2o with seem to get nice orange/yellow and can be recrystallized.
and all the other NP naphtha swim washed with water with a pinch of sodium bi carbonate
and its in the freezer now

now my question's what would have made the naphtha so blackish?
to my impression swim dint do much els then before.
and can you was dmt base with dh2o?
to my science yeah but never read it some where.
and jugle also doent dissolve in water right?

many thanx
 
Du57mi73
#2016 Posted : 5/31/2014 10:39:43 PM

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just-yb, when you add bark and lye at the same time the bark breaks down into microfine particles that float in the naptha and cause it to be brown/black. Your best way to fix this is to re-x. A soda carb wash wont really fix it. The black IS plant matter, so maybe you can try filtering it through a coffee filter, that actually might be better than a re-x.

Next time make sure you add lye and let it completely react with the water AND cool down before adding your bark. The bark you have is low quality.
"I am cursed by the blossoming knowledge of my feminine ideal and she looks suspiciously like you."

"Everybody is a genius. But if you judge a fish by its ability to climb a tree, it will live its whole life believing that it is stupid." -AE
 
sarek
#2017 Posted : 6/1/2014 3:13:44 AM

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decibel,

It sounds like what you are referring to as "plant oils" are actually contaminants from your basic solution that ended up in your final product. Through your admitted carelessness (no offense, we've all been there Wink, you mistakenly siphoned some into your collection jar when trying to separate your solvent from the aqueous layer.

If this is the case:

They are NOT good for changa. Do NOT consume them. Seriously don't.


It was smart to do a sodium carbonate wash on your product, which I am assuming consisted of dissolving sodium carbonate into water and then adding your product to the solution. The impurities that you accidentally brought from the aqueous layer will dissolve in the water, but your freebase DMT will not, so it was a good move.

When you say you "kept the oils", I assume that you kept the sodium carbonate/water solution that you had washed your spice with, and you didn't pull every last drop of solvent off the top, probably out of wanting to be careful not to pull any of the aqueous layer (also a good move).

Leaving solvent in the jar with your aqueous solution for long periods is usually only a bad idea when you are working with the filtered, basified solution from the original acid soak of the plant material, because the longer it sits, the more it will start to suck out things you DON'T want.

This is not an issue with the sodium carbonate solution, as you will not be able to end up with more impurities than your product originally had. Feel free to siphon off the naphtha in this jar without worry, but for the sake of scientific rigor, I would likely keep anything that precipitates out separate from the rest of your spice.

I've personally let naphtha sit in a jar with my original basic solution for several weeks. What precipitated out was noticeably less pure than pulls done in a timely manner, but nothing dangerous, and nothing you can't clean up.
 
JisforJohnathan
#2018 Posted : 6/1/2014 12:07:27 PM

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hypothetically, after doing an entire a/b extraction, during the step where I would wait for my naphtha, and acacia solution seperate but before I take out the naphtha to chrystalize, would there be 3 layers or 2.

the 3 layers would they be naphtha, acacia solution, and an aqueous layer.

or

would it be 2 layers one naptha and one acacia sulution.

just a little confused
 
3rdI
#2019 Posted : 6/1/2014 12:09:42 PM

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You want 2 layers, if you have 3 then you probably have an emulsion layer
INHALE, SURVIVE, ADAPT

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JisforJohnathan
#2020 Posted : 6/1/2014 12:18:22 PM

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so after mixing the naphtha, lye, and acacia solution all u do is wait for the naphtha and acacia seperate and siphon off the naphtha? In the teks I don't see where they specify. I had read that there will be a water layer below a layer of
naphtha an that that's where the lye is absorbed. and to obviously avoid the water
 
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