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Tek mash up ... here are the results Options
 
dmt005
#1 Posted : 1/16/2011 5:39:02 AM

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Ok so it has been a while... Swim has been a busy little girl and has gone through and around many obstacles and is still hitting one inperticular.

Ok I will start off by describing what SWIM has told me she has been doing and experimenting with. Ok so SWIM told me she wanted to try and mix 2 teks and see if she got an improvement in her yields. She took the â– PanoraMIX European AB and â– Marsofold's tek and kinda mashed em up and tried to put a twist of her own on it.

Ok so this is how SWIM described her tek to me.

She would take 100g of MHRB put in 400ml of acetic acid and let it sit for 2 days, after 48 hours had passed she would put it on high in her crock pot for 2hrs. After 2hrs she poured out the vinegar and repeated this 2 more time. She would then combine all vinegar cooks with the MHRB plant matter in one container.

Now she took 400 ml of H2O and added 50g of NaOH once the NaOH dissolved she poured it in the acetic mixture. This was adjusted until the PH was around 13-14. At this point she would let the mixture sit for at least 2hrs to let all the spice convert to freebase.

Now she would take her Naptha and pour 100ml into her flask and let it set on high in her crock pot until nice and hot. This was added to the MHRB soup gently rolled around for a few minutes and then removed with a turkey baster. This was repeated at least three times some times 5.

She would then reduce her pulls to about 1/4 of its original volume and then put it in a flask heat it while she was making her Na2CO3 solution. She made sure that the carbonate solution was a basic solution ( at least 12 but she tried to get it at 13 ) then she poured it in her flask containing her pulls. This was shaken vigorously to clean her naptha as much as possible, the 2 layers were then separated. Now that she washed her Naptha solution she let it set and evaporate until she had nice clean spice.

Purity is wonderful however out of 300g of MHRB she only yielded 1.3g

She is extremely frustrated and does not know what she is doing wrong and why her yields are so horrible.
 

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dmt005
#2 Posted : 1/17/2011 5:41:54 AM

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30 views and nothing.... Hmmm hopefully some feed back will be posted soon SWIM is getting frustrated trying to figure out what she did wrong.
 
Ljosalfar
#3 Posted : 1/17/2011 6:01:37 AM

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Not sure what is off, but try -
More/larger volume pulls; ***
Try freeze precipitating - then SWIY can recycle the solventSmile
Try shaking the MHRB basic + naphtha mix vigorously - at SWIY's pH it will separate
Try salting out w/ FASA on Xylene pulls, for oral doses

Lastly, 1.3 g ... great! Enough to explore and explore and explore!
L
"The first principle is that you must not fool yourself, and you are the easiest person to fool." Richard P. Feynman
 
dmt005
#4 Posted : 1/17/2011 7:12:18 PM

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Is there a possibility that HCl would result in better yields due to it being a strong acid. this would break the material down further thus possibly giving better results? How ever reports have shown that acetic acid gives good yields too....
 
Shaolin
#5 Posted : 1/17/2011 7:20:47 PM

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I think Ron69 reported that undiluted (actually 10% and more) HCl has a negative impact on the yield.

I suspect that low yield could be due to low amounts of the solution used in the first step, since you use a ratio of 1:4 (mimosa:liquid, in your case mimosa:vinegar) while 1:10 is more common, so for 100g of the bark you would use 1000ml of acidified water (or vinegar if you wish, Black Sheep say the choice is yours. Nas too. Ooop, he's talking about the world.) per cycle.
Got GVG ? Mhm. Got DMT ?

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endlessness
#6 Posted : 1/17/2011 7:53:46 PM

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where is the bark from? did you extract from the same batch before and if so what were the yields?

How many pulls did you do so far? How did you retrieve the dmt from the mix, freeze or evap?

Maybe add more lye, do another 2 pulls and see if you can get anything more. Also you can use a solvent such as limonene or xylene after. Just salt with FASI or FASA (respectively).

Hopefully you didnt throw the mimosa mix away already..
 
dmt005
#7 Posted : 1/17/2011 10:26:45 PM

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Well all pulls have resulted in around the same amount, roughly 300 mg per 100g of MHRB.
The last amount taht SWIM has been working with is still around however the reported 1.3g batch of 300g is now gone. However the batch that SWIM did with 300g of MHRB she did 5 pulls of about 100ml of naptha.


MHRB was from http://www.adenium.com.br/mimosa_products.asp.
 
endlessness
#8 Posted : 1/17/2011 10:41:25 PM

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If the last pull was yielding as much as the first pull it means that there is still plenty of dmt. When the last pulls start yielding very very little, it means its closer to end (but at this point you could still pull with a bit more polar solvent like xylene/limonene and get quite a bit more dmt out).

So basically you discarded your dmt down the drain Sad Next time keep pulling until nothing comes out. 5 pulls might not be enough
 
Shaolin
#9 Posted : 1/18/2011 3:01:38 PM

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There are no mistakes, just experiences. That being said, up the water volume.
Got GVG ? Mhm. Got DMT ?

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dmt005
#10 Posted : 1/19/2011 10:30:51 PM

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Up my water levels? Really? As said I usually do a 400ml acid cook so with a 100g batch I end up with close to 2000ml after adding the NaOH solution?
 
dmt005
#11 Posted : 1/19/2011 10:32:14 PM

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endlessness wrote:
If the last pull was yielding as much as the first pull it means that there is still plenty of dmt. When the last pulls start yielding very very little, it means its closer to end (but at this point you could still pull with a bit more polar solvent like xylene/limonene and get quite a bit more dmt out).

So basically you discarded your dmt down the drain Sad Next time keep pulling until nothing comes out. 5 pulls might not be enough



Hmmm I usually put all of my pulls together and then evap to obtain spice. I usually (have never) done it pull by pull. I have always added my pulls all together, washed and then evap
 
endlessness
#12 Posted : 1/19/2011 10:48:22 PM

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well you can still do that if you want but before throwing away the mimosa, do at least one long thorough pull and evap/freeze separate, to know if theres still dmt coming out. If there is, keep doing more long pulls or go for limonene/xylene
 
vampir
#13 Posted : 1/20/2011 1:14:26 AM

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Honestly, I don't understand all the extra (unnecessary, imo) steps. That is quite a low yield.

Some of SWIM's observations:
1. Heating/boiling/doing anything to the initial vinegar bath does NOTHING for your yield. Personally, just add some vinegar, add some boiling water, until it's partly mushy (not too liquidy though), and let it sit there. Don't touch it. Letting it sit for 20 minutes, or for 2 days hasn't made much of a difference.
2. Why are you not freeze precipitating? From everything I've read, evaporating is not good because you will have impurities enter into the spice that way. Freeze precip is the cleanest, SWIM has had snow white crystals from doing this, without having to do any carbonate cleanings of the naphtha. Pull and then straight into the freezer.

My theory on where you are going wrong, if I understand this correctly.
Quote:
She would then reduce her pulls to about 1/4 of its original volume


This seems to be where the problem MAY lie. There's a limit to how much spice naphtha can hold. SWIM has found that using around 350ml of naphtha will result in anywhere from 700mg-1000mg of spice in that pull, depending on how much it's heated. If you reduce 350 ml to 100 ml, then your "carrying capacity" will be greatly reduced - maxing out at like 300-400mg. My only guess is that some of it is escaping into your Na2CO3 solution. I've never heard of this carbonate wash step, so I don't really understand it's purpose, but that might be the culprit too. Try not to evap your naphtha or "reduce" it. It's quite an unnecessary step, and you will lose so much naphtha that way. This is coming from a SWIM who gets consistent 1.5% yields of N-N-spice.
If you insist on doing it your way still, next time try not reducing it to the 1/4 volume of naphtha. Try not reducing your naphtha volume AT ALL. Keep it at the same level, then freeze precip, and I'm pretty sure your yields will go up, but that's just my guess.

EDIT: SWIM actually did a 300g MHRB extraction recently and got 4.4g of goodness. Still has the bark laying around, should be more in there.
 
Shaolin
#14 Posted : 1/20/2011 10:07:26 AM

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dmt005 wrote:
Up my water levels? Really? As said I usually do a 400ml acid cook so with a 100g batch I end up with close to 2000ml after adding the NaOH solution?


Fo' real son.

For 100g, 3*1000ml and the reduce to 500ml.

The math doesn't do me right. 3*400ml is 1200. You use 800ml for your NaOH solution ?

vampir: He/she didn't use water, therefore he heated vinegar (instead of water). Sdoium carbonate step is to remove any possibly NaOH in naptha.

If naptha would become too saturated with DMT wouldn't it precitipate out ?
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dmt005
#15 Posted : 1/29/2011 8:52:20 PM

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I'm sorry to ahve caused any confusion. When SWIm reduces her naptha pulls what she means is that when she has done all of her pulls which she puts together in one container she then reduces the volume of naptha.

her highest Naptha pull she has ever done was maybe a little above 100ml's. To her understanding this was a sufficient volume of naptha.

Has far as the xylene option, SWIM has come to the conclusion that she hates xylene. It smells horrible and stinks up the surrounding area. The last time she used xylene it didn't seem like she had much more of an improvement on her yields.

SWIM has also thought that maybe some of her spice has escaped into the sodium carbonate wash so she keeps the wash and does a very very hot naptha pull on the wash itself to see if she gets anything ( she gets nothing from this, the pulling of the sodium solution was more of an experiment and resulted in nothing)

SWIM would also like to say that she has all of these "unnecessary" steps because as mentioned before this is a mash up of 2 dif teks in the wiki. A simple experiment that does not seem to be going to well

SWIM only wishes that she could achieve even a 1% yield.... that would be fantastic and reduce frustrations. She has given up on thinking at this time of reaching the 2% she has been hearing so much about.

SWIM is thinking for her next go at it she might try â– Shaggy's Jungle Tek as this tek is reported to get 2.2g per 500g, which now that she thinks about it is not much better than what she has been getting but it is still better.

Long story short ..... she is just getting frustrated and wants to find something ( A/B ) that she can get good yields with
 
vampir
#16 Posted : 1/30/2011 7:12:03 PM

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q21q21's A/B tek has never failed SWIM's across the globe! Razz
 
Shaolin
#17 Posted : 1/30/2011 8:37:33 PM

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dmt005: Do you have access to limonene/calcium carbonate ? If so, use q21q21's TEK.
Are a few hundred grams of NaOH viable for you ? If so, use Noman's or spice's () STB TEK.
If you want to use an A/B, well we can work something out.

Which solvent are you using ? Brand, MSDS.

Where is your bark from ? Did you discard this batch ?

I still think your yield is low because of the lack of water in the first step.
Got GVG ? Mhm. Got DMT ?

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dmt005
#18 Posted : 1/31/2011 6:08:16 AM

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This is where SWIM got MHRB
http://www.adenium.com.br/mimosa_products.asp

Solvent used is Kleanstrip VM-P Naptha

The batch described above is long gone. SWIM prefers to use A/B teks instead of STB its just her preference.
 
dmt005
#19 Posted : 1/31/2011 6:14:25 AM

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She has not looked for limonene she is currently looking to see where she might get some of this other than online. She should be able to get Ca(OH)2, as this is needed for that tek. This I am sure can be achieved as it is food grade pickling lime and should be readily available at the store.......
 
 
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