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First extraction... NOTHING?

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Orion

Orion

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OG Pioneer
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Hi all!

Iv'e been researching like crazy throught this forum and the rest of the net, but i cant seem to find myself a solution.

Ive used nomans tek pretty much to the letter, but i just cant seem to yeild..... well.... anything! After my freeze precipitations yeilded only cloudy naptha, i couldnt really figure out what had went wrong. I left it in there untill morning, from about 9 oclock the night but got literally nothing with every pull. The zippo evaporated fine on its own (though I did only test a small amount). Now I will be using Newport lighter fluid as others on the forum have reported success with it.

I evaporated all the zippo pulls together in a pyrex dish and I'm left with some very strange leathery, earthy smelling clear film, it's like a syrup that won't evaporate.

I could probably redissolve this in a small amount of naphtha and freeze that (it would be quite saturated if there is DMT in there).

Id much rather not have to do this messy evap stuff.... My freezer doesnt seem all that cold too, is this a mahor issue? does it HAVE to be super cold? it's a bosch fridge-freezer on the coldest setting. Even super freeze yeilded nothing... just cloudy naptha..... what's going on?

If the freezer DOES need to be colder, if this is the problem, anything i can do? packing it would help insulate but I'm not sure it would actually DROP the temperature much.... and getting f
dry ice is a bit of a nightmare, as i'd just lose it quickly wthout a deep deep freeze.

I have heard of people putting pulls in the fridge first, and getting crystalization, then putting it in the freezer.... so does my freezer temp matter so much?

Dammit... I was hoping to report my first experience this week too....

Can anyone suggest anything? Bit of a nightmare! I'll post results of the test evaporating some Newport fluid before using it.
 
Is your freezer a separated unit or part of your refrigerator ? (a "real" freezer or deep freezer will go down to -20°C, a 48-72h conservation one will only go down to -5°C, you may also
check how many stars it has, it is an indication of how cold it can get)
If you only get cloudy naphta it means that it isn't saturated enough at that temperature, you should evap down your naphta to at least 50% of what you currently have
then but it back in your freezer.

By the way did you pull at room temp ? Some naphtas need to be hot in order to pull efficiently.
 
Thank you. I have absolute faith in the nexus. I love the lot of yas!

That newport stuff evaps really clean by the looks of it.
 
justine said:
Is your freezer a separated unit or part of your refrigerator ?
If you only get cloudy naphta it means that it isn't saturated enough at that temperature, you should evap down your naphta to at least 50% of what you currently have
then but it back in your freezer.

By the way did you pull at room temp ? Some naphtas need to be hot in order to pull efficiently.
Click to expand...

Initially I didnt heat it before pulling it, then tried the same naptha back in, heated it all in a hot water bath, pulled again, froze, got nothing again.

*edit* my freezer has a 3 star rating, it's the lower part of a Bosch fridge freezer. Not just a compartment, the top door is the fridge, a metre high, the lower is the freezer, also about a meter high.

I'll try evapping the new fluid down first after pulling, then freezing.
 
ORION said:
justine said:
Is your freezer a separated unit or part of your refrigerator ?
If you only get cloudy naphta it means that it isn't saturated enough at that temperature, you should evap down your naphta to at least 50% of what you currently have
then but it back in your freezer.

By the way did you pull at room temp ? Some naphtas need to be hot in order to pull efficiently.
Click to expand...

Initially I didnt heat it before pulling it, then tried the same naptha back in, heated it all in a hot water bath, pulled again, froze, got nothing again.

*edit* my freezer has a 3 star rating, it's the lower part of a Bosch fridge freezer. Not just a compartment, the top door is the fridge, a metre high, the lower is the freezer, also about a meter high.

I'll try evapping the new fluid down first after pulling, then freezing.
Click to expand...

You should also check the ph of your mhrb mix, if it is too low you won't pull much.

edit : and by the way, where did you buy your mhrb ?
 
Another though : If you have a 1:1 mhrb:lie ratio you can shake the hell out of your jar when pulling, there shouldn't be much emulsion and you will be able to
recover all your naphta after less than an hour.
 
Thats quite true, i find I can be very rigorous with the shaking and the emulsion/ fine bubbles ALWAYS settle right down within about 5 minutes. Also I heard my mimosa supplier is a sponsor on the nexus... This true?
 
Oh and since you live in la perfide albion you might be glad to hear that you can order all kind of cool solvents from this uk based shop.

DCM, although quite toxic, is extremely efficient in pulling dmt (only one pull is needed to get nearly everything) and after it is evaporated you can
purify your dmt with a naphta freeze precip.
 
If i can just figure out whats goin on here, and get it to work, i plan to use DCM next, seems much more reliable. Even though it sinks to the bottom... hmmm
 
ORION said:
If i can just figure out whats goin on here, and get it to work, i plan to use DCM next, seems much more reliable. Even though it sinks to the bottom... hmmm
Click to expand...

Well, since you need only one pull with dcm you can filter your bark and use a sep funnel to get it.
 
ORION said:
Ive used nomans tek pretty much to the letter, but i just cant seem to yeild..... well.... anything!
Click to expand...

Noman's been my first extraction. It's yielded ~1% on my first attempt. It is pretty much fool-proof.

Only things that come to my mind are insufficient reduction before freeze-precip or insufficient basification. Did you check your basic solution pH?

ORION said:
I evaporated all the zippo pulls together in a pyrex dish and I'm left with some very strange leathery, earthy smelling clear film, it's like a syrup that won't evaporate.

I could probably redissolve this in a small amount of naphtha and freeze that (it would be quite saturated if there is DMT in there).
Click to expand...

I would suggest doing a mini-A/B on the evaporated extract. That's if you have some spice in there.

ORION said:
.... My freezer doesnt seem all that cold too, is this a mahor issue? does it HAVE to be super cold? it's a bosch fridge-freezer on the coldest setting. Even super freeze yeilded nothing... just cloudy naptha..... what's going on?
Click to expand...

Well, once my NP solvent is properly reduced, the spice starts to crash out even at a room temp. Most of the spice is out of the sultion in the fridge (~0C). So, either the spice is not there, or your solvent is not sufficiently saturated.

ORION said:
I have heard of people putting pulls in the fridge first, and getting crystalization, then putting it in the freezer.... so does my freezer temp matter so much?
Click to expand...

Mine is around -15C at best and I do not need more (tested by evapping residual naphta).

Oh, well. I use lab grade heptane or hexane instead of lighter fluid.
 
I didn't get to cheack the PH, but I used 5og of lye to 50g mhrb to 750ml water. Added water to a large glass jar first, then 50g of lye, let it dissolve and cool to room temp, the added 50g of powdered purple/pink mhrb, (which took some mixing in, as it doesent sink so well when dry). Mixed well, then let it sit for about an hour and a half, then started with the naptha pulls.

These naptha pulls with the new fluid don't seem to be doing anything new. I'm evapping it down all together, to about 50% Then i'll put that in the freezer.

Just not expecting anything much.... If i I evapped the other pulls together, I should have got at least SOMETHING but... nope.
 
Hmmm... I think your zippo lighter fluid might be a new substitute that doesn't pull much, check its EINECS reference. Also, in the future do not use zippo lighter fluid since it's quite expensive (at least where I live, across the channel, it's about 8E/l whereas generic light odorless naphta is only 3-5E/l).
 
There are very few things that could go wrong with this tek.

ORION said:
I didn't get to check the PH,
Click to expand...

Are you absolutely sure your lye is of good quality? I would definitely start from checking the solution pH. If you basify the solution to pH over 13, then the spice would have nowhere to go but to your naphta.

ORION said:
... then let it sit for about an hour and a half, then started with the naptha pulls.
Click to expand...

I've soaked mhrb for much longer, like 12 to 24 hours.

ORION said:
These naptha pulls with the new fluid don't seem to be doing anything new. I'm evapping it down all together, to about 50% Then i'll put that in the freezer.
Click to expand...

I reduce my NP solvents to 10% - 20%. Try it.

ORION said:
Just not expecting anything much.... If i I evapped the other pulls together, I should have got at least SOMETHING but... nope.
Click to expand...

Your spice did not go anywhere, that is if it was in the bark in the first instance. But you say it is from pedro, than it should be OK.

Good luck.
 
Ok I tried reducing my solvent down to 40% after 3 pulls of about 37ml (using a glass bottle with a thin stem, easier to suck it all up without the base solution entering my squeeze bulb/ink syringe thingy). The 3 pulls where added together in a jar, evapped down, and stuck in the freezer.

I woke up to some little crystal formations, so i poured off the naphtha through a coffee filter and reused it to do some more pulls, and I added the syrup yeild from before to this naptha after the 3 pulls, sodium carbonate washed it, sucked it back off the top, evapped it down to 40% and put that in the freezer too.

Technically speaking this is 3 sets of 3 pulls. The first one I resorted to completely evaporating and yeilding syrup, then these two. This is all from 50g of bark.

I plan to recrystalize the full yeild too.

Next time I'm going to do all this at once with triple the amount, with another 100g of bark added to my remaining 50. 150g MHRB, 150g NaOH, 2250ml water and 450ml naphtha total (naptha will be used evenly as before, this will be done in 3 bottles all at the same time, precipitating in 3 jars a a time in the freezer).

Will these volumes work (just tripled from before) ? I want to use a method that involves less fussing about this time, if possible, because this whole thing has sucked up quite a lot of time so far...

But thanks guys! Now I have a result! <3
 
ORION said:
Ok I tried reducing my solvent down to 40% after 3 pulls of about 37ml (using a glass bottle with a thin stem, easier to suck it all up without the base solution entering my squeeze bulb/ink syringe thingy). The 3 pulls where added together in a jar, evapped down, and stuck in the freezer.
Click to expand...

Usually I do 5 pulls 20 ml each and reduce combined pulls to 15-20 ml. That is for 50 g mhrb.

Do not be afraid to suck up some of the base solution. It is easily decanted later. Buy a sep funnel. It saves so much hassle. I bought a 500 ml one with teflon stopcock for $30.

ORION said:
Will these volumes work (just tripled from before) ? I want to use a method that involves less fussing about this time, if possible, because this whole thing has sucked up quite a lot of time so far...
Click to expand...

A sep funnel, a pH meter, and a distillation setup (if you do not want to waste your solvents) would help a lot.

Experimenting is half of the fun for me. I am doing small-scale extractions mostly, always trying different things.
 
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