Extraction question ( seperation )

[Raziel]

If I were to have a 2 litre jug full of basic MHRB solution and it is seperating very slow unless I super heat it and then it seperates at a reasonable speed.

Can the jug of liquid be halfed and then toped up with basic H2O ?

It doesn't seem to be too thick and only 250g of powder was used but it just seems really slow to seperate.

What would you do ?

[Thre365ive]

A lot of times if you just add more NaOH it'll help. How much water and lye did you use?

[Norman]

Yeah, some quantities would help. STB? A/B?
Adding water definitely won't hurt. Adding 6og of salt per liter of solution could help too. I'd do both before adding more lye if you're sure your pH is 13+.
What kind of NP?

[dimension traveler]

yea I would defanantly half and add cooled down basic h20. adding straight lye to solution is what we call spikes, it will most likely get some parts to hot and break down the spice, resulting in a loss of yeild.

[Raziel]

What would the signs be if I have "broken down" the spice with excessive heat, how could I tell ???

[bbd2]

unusually low yield

[Raziel]

Ok so I know the first 3 pulls were not fried because I combined the three pulls and started to evaperate in a dish. I have a MASSIVE cluster of crystals forming in the corner. It probably the size of a 2p coin and hard/brittle to touch. Not fully evaperated yet so don't want to probe it too much.

I am going to split the volume in half and top up with basic H2O. Hopefully it will seperate better with out too much heat being applied, that's if I haven't fried the remaining spice.

[lysergic]

Originally Posted by Norman

Adding water definitely won't hurt. Adding 6og of salt per liter of solution could help too. I'd do both before adding more lye if you're sure your pH is 13+.
What kind of NP?

Good advice.

[dimension traveler]

3 pulls already, were they small? It's ok to do heat baths, probally wont burn them doing that, and slower the seperation the better, for me when I do a heat bath I just run hot tap water over my jug and it takes like 20 min to seperate. adding the lye straight to solution like I said about the spikes is where you will toast the spice. good luck

[whatchamacallit]

One can add straight lye crystals to the solution without harming spice. This allows one to not add much to the volume of the aqueous solution. No one has ever proved that alkaloids are damaged by adding straight lye, and to the contrary, SWIM has done both ways without hurting yield at all, so this is just a rumor. SWIM would suggest the heat bath, and adding enough lye (pH as close to 13.5-14 as possible) and water (enough water that the solution isn't thick and sludgy) to help separation.

[dimension traveler]

you could add if you do slowly. spice in it's freebase form starts breaking down at 140 degrees ferenheight. so yes if you were to add fast that temp could easily be reached. and I have lost spice heating to that temp.

H20 can hold quite abit of lye if you saturate it.

[cars2024]

nap doesnt like bases at all so if its taking more than say 15 min to split your not high enough on the PH meter.. add another teaspoon of lye

lighter fluid has a chemical added to it which is suposed to reduce evaporation and odor when burnt.. i've noticed that lighter fluid tends to take a bit longer to split due to this oily chem you may wanna try to get some naphtha used as paint thinner (Ace Hardware VM&P Naphtha Pure) is the best i've found

[Raziel]

Originally Posted by cars2024

nap doesnt like bases at all so if its taking more than say 15 min to split your not high enough on the PH meter.. add another teaspoon of lye

lighter fluid has a chemical added to it which is suposed to reduce evaporation and odor when burnt.. i've noticed that lighter fluid tends to take a bit longer to split due to this oily chem you may wanna try to get some naphtha used as paint thinner (Ace Hardware VM&P Naphtha Pure) is the best i've found

We have a hard time in England trying to find what the U.S. call Naphtha. Ronsanal lighter fluid defintaly works to a certain extent. I used it to extract bone dry light yellow spice.

Regarding this extraction though,

I have got 5 g yeild with 1 maybe 2 more pulls left to do. I think I used 300g and not 250g as I split the bag using sight only and this batch of powder felt a lot heavier. The problem I have is the yeild is much yellower than my first attempt almost a light orange. Doesn't feel oily at all but it tends to clump together like there is moisture present which is why I think there maybe a tiny amount of oil present.

Is there anything I can do to get the absolute bone dry and as it is at the moment is it safe to smoke ?

[dimension traveler]

pics always help, but you could just spread it out on a plate or something and hold next to a heater, just dont let it get to hot.

i've seen the more yelllow orange stuff 2 from when I did a stb and not a/b and it does seem sometimes that it has moisture/oil. rex's never hurt.

but anyways as long as you dont smell any np, lighter fluid in your case in there and just that good ol spice you should be fine to smoke.
Happy Journeys

[Raziel]

Heres some pics. The lighter stuff is 3.7 grams form my first extraction (3.7g after smoking A LOT one weekend) and the darker stuff is 5 g from this extraction. As you can see it is not as powdery as the lighter stuff but they smell exactly the same.

Also, maybe the supplier sells really good quality pre-powdered root bark or the % of DMT isn't quite right, I have gor approx 8.5-9 grams from 500 grams of pre-powdered ???

Any way, how does it look ?

[whatchamacallit]

A quick heptane recrystallization can clean the oily color from the DMT.. Those pics look fine, but be sure that it sits out in front of a fan until it's totally dry. If you smell naphtha when that bag is open, then it needs to dry more. A heptane recrystallization could turn that yellow waxy stuff into pure white/clear crystals in probably one attempt.

One just heats heptane to close to boiling, then adds it slowly until all the DMT just dissolves. As it cools, the DMT will begin to crash out again. If there is a yellow/orange layer that drops out first, the remaining cloudy/milky white solvent can be decanted from the top into a fresh dish, and this will give white DMT. If yellow/orange does not begin to fall out first, then one can just let the solvent freeze, and the DMT should all recrystallize in the bottom of the container, and the solvent can be poured off, and left to evap the tiny bit left on the crystals to leave a much cleaner/more pure product.

If the yellow/orange layer separates from it, one can repeat the recrystallization on the colored goop to pull out more DMT, and this can be repeated until one is sure they have all the DMT out.

[Raziel]

where would I get heptane ? How about a "ammonia wash" I know a store that sells the 10% stuff.

[whatchamacallit]

Ammonia wash won't clean out much color, if any, and can cause loss in yield. It's better to do a polar wash on the solvent before the DMT is crystallized, like in SWIM's tek.

Heptane is known as bestine (brand name) in the states, but not sure about how to find it in other countries, besides ordering it off the internet. It's not a watched chemical or anything, so one could probably order a gallon, maybe less, and have it for years to come for plenty more DMT projects.

[Raziel]

What is it used for whatchamacallit so I can try and find the British brand name ?

[dimension traveler]

the heptane that he is reffering to is a rubber cement remover, I always find it in art supply stores

sorry whatchamacallit no adfense but imo you dont wont to get it close to boiling. I have done this many times and have lost alot for going to high in temps. the spice strarts breaking down at 140 F. try not to go any hotter than that to desolve it all. 150 is as hot as you should go if you use 30 ml per gram of spice.

and to make it so that the impurities fall out first you have to come up with a way to make it cool down real slow. THeres better ways but I usually use a mason jar then as soon as i take it out of a heat bath I wrap lots of seran wrap around it and put it into a cooler then fridge and finally freezer. I dont decant at all. it's easy to scoop the good and leave the bad behind if you stand the jar on a 45 degree angle.

[whatchamacallit]

SWIM just lets it sit at room temp and the orange layer begins to drop out, especially when recrystallizing a decent amount. SWIM prefers to pour the milky solvent into a new dish, rather than scrape the white crystals off the goo. It also crystallizes faster, and then one can repeat the process on the orange stuff again to pull out more DMT. This can be repeated until one feels they have all the DMT out.

[bbd2]

Originally Posted by dimension traveler

and to make it so that the impurities fall out first you have to come up with a way to make it cool down real slow. THeres better ways but I usually use a mason jar then as soon as i take it out of a heat bath I wrap lots of seran wrap around it and put it into a cooler then fridge and finally freezer. I dont decant at all. it's easy to scoop the good and leave the bad behind if you stand the jar on a 45 degree angle.

ime this way works better than the technique where you decant and leave the colored layer behind

my dude , instead of the saran wrap-> fridge-> freezer slow cool
he leaves his in the heat bath for at least an hour
lets it cool so it dont crack in the freezer
then puts it in the freezer for 24-72 hrs (12-24 hrs for the early precips, 72+ for the last one)

very white dmt forms on top of the colored impurities

the white is easy to scrape and recover

while the colored impurites are sticky and hard to scrape,
so you dont

filter the heptane,
put it back in the jar
reheat in the heat bath
and repeat the freezer step

until its done (youll know when, usually 2-3 times)

for me, non-rex'd spice is too harsh to vape off glass

[Raziel]

I have been looking for a while over the net trying to find any mention of heptane in the UK and I don't think they sell it No sign of it in art supply stores either ...

[dimension traveler]

Did you use napths for your non polar? you could use that as well, wont get it clear but can get it white after a couple goes.

[Raziel]

Originally Posted by dimension traveler

Did you use napths for your non polar? you could use that as well, wont get it clear but can get it white after a couple goes.

Napths for non-polar ??? I don't understand. I used lighter fluid which is the equivalent to naphtha.

Are you saying the extraction can be dissolved in lighter fluid to clean it up a little ???

[Raziel]

I have been thinking of what dimension traveler said and I have a question. The impure extraction I did was probably because I did not freeze precipitate but instead evaperated the whole of the "Naphtha". Can I chuck the yeild into some warm Naphtha and then freeze precipitate the DMT resulting in cleaner spice ?

Will this work ???

[Thre365ive]

Originally Posted by Raziel

I have been thinking of what dimension traveler said and I have a question. The impure extraction I did was probably because I did not freeze precipitate but instead evaperated the whole of the "Naphtha". Can I chuck the yeild into some warm Naphtha and then freeze precipitate the DMT resulting in cleaner spice ?

Will this work ???

Yes, but you'd be better off performing a proper recrystallization. Put the DMT in a small shot glass or something. Warm the naptha, then add it to the DMT dropwise while stirring until just the DMT dissolves and you have some yellow goo at the bottom. Carefully decant off the naptha, and let it slowly evaporate or freeze precipitate it. Save the yellow oil for infusion onto some kind of smokable leaf.

[dimension traveler]

yes you should be able to use the lighter fluid but it wont be as good as the heptane. try doing the precip first, cause it's so easy should clean it up a bit, then do the recrystal, can use the same methods that we told you useing heptane as the example.

[Raziel]

Thanks guys but I have a question.

If I drip warm naphtha on to the extracted spice just untill it has all dissolved, wont I just end up with a gooy blob which I imagine would be hard to freeze precipatate. If the solution is too thick wont the good stuff find it hard to precipatate ???

[Thre365ive]

Originally Posted by Raziel

Thanks guys but I have a question.

If I drip warm naphtha on to the extracted spice just untill it has all dissolved, wont I just end up with a gooy blob which I imagine would be hard to freeze precipatate. If the solution is too thick wont the good stuff find it hard to precipatate ???

Nope. Just keep dripping it till it's liquid. As long as it stays hot, you should be fine. Try putting the flask with the spice in it in a hot water bath to be sure it stays warm.

[Raziel]

Shpould it all be liquid ??? I am in the process now and I have a ornage goop at the bottom in warm naphtah, shoudl I add more untill it dissolves ???

[Raziel]

How do I know when all the DMT has dissolved ?

Here is what I have done so far. I put the orange dmt in a glass that is in a dish of hot water (hot water bath) an I slowly added the hot naphtha. It slowly dissolved and I noticed the naptha was turning yellow like in the intial extraction and a cluster of dark orange crystals were sitting in the bottom. The more naptha I added the more they dissolved. I stopped adding naphtha when the dark crystals started to dissolve and decanted of the naptha leaving the crystals at the bottom.

I put the yellow liquid I decanted off into a tray and left it at room temp. I noticed alot of blobs of dark ornage junk had settled to the bottom so I decanted it again into a clean tray and now the tray is sitting in my freezer.

Is this all ok at the moment ?

I am left with a glass full of dark gunk from the intial clean up and also a tray full of the same colour (dark orange) gunk that crashed out the first decant.

Should I collect all the "gunk" together and repeat the above ?

Please help, im really unsure about all this and if I have made any mistakes or not.

Thanks you

[piggy69]

Hello again Raz. Its always difficult to know precisely what to do until youve done it a few times and even though every one is trying to help it can get confusing very quickly.

Heres what I would do with UK materials in mind but wouldnt because it is illegal
1- Get yourself a clean jam jar and quarter fill with ronsonol lighter fluid
2- place all your product into the jar with the ronsonol and put into a hot water bath straight from the kettle. This should disolve everything into solution. If it all hasnt dissolved add a small amount more naptha till it does. This will make sure that the solvent is holding as much spice as it possibly can.
3- Place the jam jar with the lid on into the bottom of the freezer and leave it there a good few hours.
4- Put a coffee filter inside a funnel and put that in the freezer too to cool it to the same temp.
5- Pour the crystal full liquid through the filter into another jar/glass leaving all the goods in the filter.
6- Let the whole filter "dry" until no smell of naptha can be detected
7- Get some of the 10% houshold ammonia solution from the paint shop/BQ etc. and put that in the freezer for a few hours and then pour about 2 shots worth of very cold ammonia over the crystals. This will take alot of the yellow/orange colour away and leave you with a much smoother smoke. In my friends experince you hardly lose any goodies and the crystals that are left are top quality!!! (Whatch the fumes they make you gag)
8- Let the filter sit somewhere safe till no more smell of ammonia can be detected.

Optional:

9- Take your product and put in a shot glass.
10- Pour on a small amount of Acetone (which you can get on ebay) until it dissolves.
11- Add twice as much herbal matter such as Mullein, Blue lotus, Pao d'arco to spice and let the acetone evaporate. You then have CHANGA which is a much nicer ride. The different herbs can add totally different experiences with the pao d'arco being the most pleasant so Im told.

Good luck!
Piggy

[Raziel]

Thanks for the advice piggy but I am already into the method I mentioned above. I will keep what you said in mind though. Thanks.

[piggy69]

No worries. Still time to try a freeze precip and cleanup.

[dimension traveler]

It sounds like your going to have some better stuff that comes out of the freezer but there may be a little spice in the gunk.

ammonia washes it good but usually imo takes to much spice away.

As you may have noticed when useing the lighter fluid or naptha, is that the spice disolves first then the impurities. It can be hard to know when you have just dissolved the spice and not the impurities.

So imo the best thing to do is:
1. know how much spice your going to wash
2. get a jar and poor 100ml LF/naptha for every gram of spice you have.
3. dump spice in
4. heat jar with solvent and spice until everything dissolves.
5. remove from water bath and either:

1. emediatly wrap with seran wrap (to insulate) set it somewhere where it wont be disturbed on a 45 defree angle, until room temp, then into fridge, then into freezer. (letting it cool that slow will allow their to be a fine line as to where the impurites and clean stuff in the jar). if properly left at an angle the whole time the impurities which are really sticky will be in the bottom corner of the jar. being that there sticky theres no problem scrapeing the clean stuff away after you have poored your solvent off. (this way you do a wash and a precip at the same time.

2. or could try to decant at the right time and just throw that into the freezer, but like i said imo it's hard to tell right when the impurities have fallen out and not the spice. (what you did)

so to wrap it up in a nut shell my opinion is to not decant, just dissollve it all and do a slow cool down then poor through fillters to catch any loose spice and scrape the good clean spice out of the jar leaving the stick impurities behind.

Maybe when your all done you could do a easy test for us that will help. see what temp the impurities dissolve at. that way we know what temp to stop at so we could do a easy clean wash by deccanting at just the right moment.

Good luck let us know how it goes.

[radical]

can anyone tell me how to properly dispose of my tek? You know my jar of purple black liquid containing h20, lye, naptha, and spice powder. I'd like to make sure I don't do something I shouldn't... but is a general drain fine with some flushing??

thanks.

[Raziel]

Originally Posted by radical

can anyone tell me how to properly dispose of my tek? You know my jar of purple black liquid containing h20, lye, naptha, and spice powder. I'd like to make sure I don't do something I shouldn't... but is a general drain fine with some flushing??

thanks.

Get your own thread but because i'm nice, just chuck it down the drain then flush with tap water.

[radical]

Originally Posted by Raziel

Get your own thread but because i'm nice, just chuck it down the drain then flush with tap water.

okok my bad sorry for hijacking your thread glad you are nice

[Raziel]

Ok clean up complete

In total I cleaned up 6.4g of oily DMT, in total I mangaed to get back 4.8g of bone dry nice yellow DMT by dissolving in warm naphtha and then freeze precipatation.

A couple of the trays produced almost white crystals and towards the end I was getting only really yellow and oily yeilds.

Heres some random pics, check out the impurites that were left over from the first few extractions. I continued to dissolve that mess in naphtha and managed to get a little more spice ffrom it. Haven't got a picture of the final gunk but it was brown oily disgusting gloop.

Heres the gunk which had the same texture as candle wax, looks clean compared to the final gunk I scrapped down the sink.



Heres some extraction pics.



Heres the final yeild from 6.4 g.



Total yield of smokable clean yellow DMT from 500g of powdered MHRB was 8 grams

[dimension traveler]

good job, bet it's a little better then before

the only thing with nathpa is that you have to wash it a few times to get it white ish. sometime if you can try the slow cool method and c what u think.

Enjoy Hyperspace

[Thre365ive]

Try it one more time, but watch your amount of solvent this time. You should need a good bit less. Should come out white after that.

[paph]

VERY nice Raziel! and a good yield too.