I was wondering if anyone might be able to shed light on my issue....? I would post in main extraction forum, but can't due to restrictions on new members.

I've run through a typical AB extraction of 1kg of MHRB. Boiled in acetic acid @ approx pH 3.
Reduced to a few litres and allowed to cool, filtered and separated from sludge.

Then basified with 50g of NaOH to pH 12 plus (pH meter struggled with extreme pH)

This was left for a week while I worked on some ACRB.

I only had 400 mL of naptha (waiting for order), so I seperated approximately 1.5 L and heated in a bath with 100 mL of naptha. This was mixed and then allowed to separate in heat bath and layers form. It looked fine, no emulsion. This was repeated with another 100 mL, and then 200 mL.

As soon as it cooled to room temp it was good and cloudy. There was a few blobs of base in the jar which I separated out when I put naptha in a dish for freeze precip.

Now this is where I notice something isn't right. It smells of NaOH or caustic soda (lye in american)

After a night in the freezer I can see normal looking DMT crystals formed on the glass and atop a layer of creamy sludge which I assume to be NaOH that has somehow got into the naptha layer. There was definatly no base solution in the dish after seperation. The creamy sludge was already in the naptha after seperation from the base layer.

What has caused this to occur? Have I over basified my initial base? Was it too hot when I separated it? Did I not leave it long enough to seperate out (unlikely as it had separated perfectly) ? Was there not enough naptha in ratio to base solution? I just assumed from my chemistry knowledge that the naptha would simply take on as much DMT as it could before reaching saturation point, then I can do further pulls when I have more naptha....

And how do I recover the DMT from the naptha now? I'm thinking of doing an acid wash to but unsure if it will work if there's NaOH in the naptha?

Any thoughts or comments would greatly appreciated

It is most likely from incomplete separation, but it's a pretty common occurrence so don't beat yourself up about it. I always do a sodium carbonate wash on my solvent before freezing. This removes polar impurities. What you can do now is, once the freeze precipitation is complete, pour the naphtha back into the basic solution for more pulls, scrape up what crystallized out, and redissolve it in a small amount of fresh, heated naphtha. Polar impurities such as lye will sink to the bottom while the DMT dissolves. To be extra careful, you could then do a sodium carbonate wash on this solvent before freezing again.

Search the forums/wiki for "sodium carbonate wash" and "recrystallization"

Ok, thanks....

On further reading I now realise the naptha and base solution was overheated.

The naptha was reheated in a heat bath then separated out the clear naptha. Then the remaining 'sludge' (is this the right term? I know people are particular about the nomenclature here) was diluted in more naptha and an acid wash was performed on this. Now the naptha is visibly clearer, then turning cloudy at room temperature. Not yellowish and then going really cloudy like it was before.

Will report on what precipitates out this time after a wash up with some Na2CO3 before going back in the freezer.

Regards,

Shambolic

The acid wash and sodium carbonate wash at warm temperature seems to have worked. Looking as it should

Newbie here... just wanna ask if anyone had extracted this kind of crystal like visually but oily to the touch? used Q21Q21 tek 2..

Depending on the quality of the naphta used, the amount of oils, waxes, NMT etc. in the plant material, the type of plant material, the rigorousness of defatting, the temperature of the extraction solvent and many other factors, the appearance of the extraction product may vary. Don't be disappointed if your first result doesn't look as good as some of the material boasted about on this forum. Fishing tales are not limited to fishermen.

Your product looks a bit wet, did you leave it to dry for a couple of days? Sometimes even light naphta contains a small fraction of heavier hydrocarbons that can take longer to evaporate. Sometimes a bit of water got suspended in the naphta and precipitates as ice in the freezer and later melts into the DMT, wetting it. Sometimes DMT is not the only alkaloid extracted and impurities make crystallization slower. Give it some more time.

Thanks pitubo, SWIM had used 125g MHRB, 125ml lime, zippo blend c 125ml, 5% native white vinegar as stated on the tek. Waited a week before extracting. The picture posted is right after the container was taken out the freezer after 24hours.
At the moment doubting every ingredient that was used...
The last ingredient SWIM hopes that is at fault is the MHRB.. It came a long way across the globe.

is it normal for the naptha to be clear when removed from the mush? Or should it at least have some hint of dicolorization other than being crystal clear?

Hi everyone im after a bit of help with 2 Different Extractions that i have ended up with 2 different results. The Extraction was from the tek (LexTek Extraction V1 )
http://www.scribd.com/do...LexTek-DMT-Extraction-v1


Shellite
caustic soda
Tank rain water
vinegar
Acacia Obtusifolia Bark
Digital Ph Meter




the mixture was left in freezer over night lots of white fluffy crystal like suspemsion floating around and some water which is the large bit floating in the third picture, I then evaporate with a hair dryer and the crystals slowly dissolved and when the shellite had completly evap'ed it ended up turning into a sticky whitish clear residue in some places alot like clear toffee and when i tried to scrape it all turned into yellow slimy substance i left in the sun to evap and it was left with no crystals that had a layer of clear sticky resin and the yellow was still really gooey and slimy







i did another pull on the basified mix and there is no where near the amount of white suspension as there was in the first freeze precip i did on first pull, i poured off the shellite and let evap in front of the air conditioner and it ended up a tacky clear layer so i put some fresh shellite in and put in a heat bath to redissolve but the sticky tacky substance would not dissolve in the shellite i then let it precip in the freezer and this is the results



2 extraction
there is these white long chunks that are not crystals and when i moved with a needle they break and as it hits the air dissolves into a sticky clump nothing like the first extraction and it was done the same way other then leaving the bark in acid step for longer and probably more heat at around 60-65 degrees during the first acid step and when using heat baths but nothing was over 50 in the mix





I have another precipitation dish that is the same extraction as above i just couldn't put all the shellite in the one precipitation dish and it has not been touched i am going to leave it for 2 or 3 days and see if there is much of a difference


Have i let my mixture get to hot in first acid stage it was upto around 65 degrees
have i let my mixture get to hot in Heat bathing during shellite pulls didnt go over 48 degrees
The first extraction i could see the the white powder forming as it hit the cold dish i was using for freeze precip and looked very good but am i ment to slowly adjust the temperature to freeze precip or is straight in the freezer ok
i have read that water oxidises dmt at around a ph of 7 is that correct if so would it affect dmt alot in freeze precip because alot of my mixes even when covered with cling wrap have had water but only a couple of drops

I have to say, your post was difficult to read. Punctuation is your friend.

It sounds like you let the crystals from extraction 1 redissolve, which defeats the purpose of freezing. You are supposed to pour the solvent off of the crystals and allow them to dry, not leave the whole solution in the sun. You basically ended up with exactly what you had before you put it in the freezer.

Your description of extraction 2 is unclear, so I'm unable to offer advice.

The word you're looking for is protonate, not oxidize. A tiny amount of pH neutral water in your dish isn't worth worrying about, it's common and rarely causes an issue IME.

Wow Yes you've certainly made a mess of things !!

Did you actually read the TEK before you've attempted it !

As Sarek said you're meant to pour off the shellite then place it I front of a cool fan to evap the small amount if solvent that's left behind , and a hair dryer is only going to melt things more so then the sun !

With you're temp problem 45 degree is the right temp for the acidifying water baths , and also you should let the base soup return to room temp before pulling with hot shellitte !

Also before the freeze stage let the pulls return to room temp then strait into the freezer is ok , You only slowly let the shellitte go from hot to freeze slowly if you're wanting to grow large pretty crystals but to just extract normal white fluff it doesn't really matter all that greatly !!

But before attempting another extraction I'd read the FAQ wiki , along with the recipe for extraction over until you fully understand what the author ( alchemist ) means !!

Hope it works out for you in the future !

i couldnt pour the shellite off after freeze precipitation as it would of also poured off the white suspension that i beleive was dmt the majority of was not stuck to the bottom after freeze precip.
Just inspected the shellite batch that was left for 48 hours to freeze precip, there was a white suspension through the shellite so it was poured through a coffee filter where it clumped in a fluffy mass at the bottom, after a few minutes it disappeared and seemed to dissolve through with the rest of the shellite. It was definitely not water ice as the shellite was captured and there was no water in it.
What's left in the bottom of the dish is very white but still very sticky.

So i had some better results on another pull i poured the shellite off after i blew on the mix for awhile and the crystals or formed a group and stuck to the glass they are still abit wet in this photo but they are alot drier at the moment i will post more photos in an hour or so
the last mix looked exactly the same that is pictured above with lots of white fluffy crystals. i just shouldn't have evaped and put a hair dryer on it and insted should have got crystals to stick and pored shellite off then evap without any heat or force of air

Ok, I'm back here again with another issue....

The first pull carried out with lighter fluid required an acid wash to get rid of some lye sludge the came through at too higher temp & yielded 2g of slightly off white goodness that was certainly an exceptable result...

However, for further pulls a 5L can of naptha was procured and appeared to leave no residue on a evap test. So further pulls were done with this naptha. First dish yielded some nice needle like Xtals, but a lot of yellow oil. So this was redissolved and sodium carbonate washed. When put in freezer, not much pricipitated. So it was evaporated and left a clear oil

It was quickly concluded that the only difference between this pull and the previous was the naptha. A larger ammount was evapped to test again for residue, and a heavy hydrocarbon greasy residue smelling of oil was observed this time around.

So, to make life easier I have got a beautiful old round glass separation funnel and fabricated a wonderful lab stand for her And some colemans stove fuel, which is known to be good and is based on heptane and pentane.

An acid wash was the plan in order to salvage whats in the rest of the dodgy naptha and to re-basify and transfer to the good naptha.
All pulls (three dishes of dodgy naptha approx 500 mL each) was evapped to approx 500 mL. Some yellow Xtals and oil were forming at room temp, and it would turn cloudy when blown on to cool below room temp (it's midsummer here and fairly warm).
This was warmed in a heat bath and filtered to remove dust.

Now when swirled (not shaken) with some pH 3 water with acetic acid a bad emulsion has occurred and is being very stubborn.
Some NaCl C2H4O2 (salt and vinegar) solution has been added to no avail.

All the info on the wiki and forums regarding emulsions is about base solutions, not acid.

A few questions about techniques to assist separation...


Will heating it cause some DMT to transfer to the naptha layer from the acid layer?

A suggestion for base emulsions is to increase the pH. Does anyone with any experience here think that doing the opposite and lowering the pH with a strong acid such as HCl could perhaps help with the separation?

Another idea is to turn this step into a defat and basify the solution to see if the solution will behave better after a defat step?

I have run out of NaOH, but have some KOH (potasium hydroxide) solution to work with. I prefer the idea of working with KOH as the base solution will not be black and stcky.

Is KOH an exeptable base compared with NaOH? It's says it's ok on the wiki, but are there any other pros or cons?

I'm aware the bonus of NaOH is that it heats the solution, but thats ok with me for the bonus of an easier to handle solution that doesn't cling to glass and everything.

Lastly there is a lot of hearsay and conflicting information in various tek's and forum discussions. Whats the exact right temperature to heat base and naptha while pulling?

Many thanks for taking time to read this and thanks in advance for any thoughts on these questions.

Edit, I just found this:

http://wilksir.com/pdf/B...l_Grease_Extractions.pdf which might be of use to anyone else having emulsion issues.

Hi

Quick background - to extract crude Harmaloid freebase I followed the EASY Harmaloid Freebase Extraction tek.

It was brown, powdery & having used it in a Changa blend, worked quite nicely.

I wanted to clean it up a little, so I followed the second part of this tek.

So,I
Mixed 50ml white wine vinegar & 150ml water & dumped the crude extract in it.
Mixed 100ml water with sodium carbonate until saturated
Mixed the solutions together.
Colour changed rapidly, as expected.

Now the confusion.

The tek says "put jar in fridge, wait a couple of hours until the yellow powder falls to the bottom"

The powder that fell to the bottom is still brown. The liquid is yellow.

Have I done something wrong, or can I filter the liquid out & use the powder?

Me again with separate issue:

For 1g Harmine HCL, to convert to freebase, I know I need to dissolve it in water, add sodium carbonate, wait for precipitation, filter.

However, my first attempt resulted in using way to much water, too much sodium carbonate, and ending up with a messy kitchen.

So the question is, for 1h Harmine HCL:
What is the minimum amount of water the Harmine HCL will fully dissolve in.
What is the minimum amount of water & sodium carbonate (base solution) I need to pour into the saturated Harmine solution to precipitate all the alkaloids?

Additionally, from 1g Harmine HCL, how much freebase (weight) should I get?

Thanks

Me again with separate question:

The question is - did I likely destroy much of my DMT by putting it in boiling water for 5 minutes?

I know you can do a fast evap of Acetone when making enhanced leaf, as the boiling point is around 52c. (put your changa mix (spice & herbs) in jar into boiling water & the acetone will boil away quickly).

Can you do the same with IPA without destroying the DMT? (the boiling point of IPA is ~ 83c), so it has to be in the heat longer

The reason I ask is:
- I usually use Acetone for making enhanced leaf.
- Yesterday I wanted to make Changa (1g dmt, 1g leaf, .6g harmalas)
- I'd read that harmalas do not dissolve in Acetone & you need to use IPA)
- I tried the fast evap with IPA. It was in the water for ~ 5mins

When trying my Changa last night, it seemed very weak on the DMT front.

So, I added extra DMT to the same mix, and it blew me away.

Did I destroy my DMT by fast evapping with IPA?
Can I just use Acetone with my Harmalas instead?

Most likely you`re ok, dont worry. Just try to smoke it and let us know how it goes.

and no, you can`t use acetone to dissolve harmalas since they are very poorly soluble in acetone.

Greetings from my kitchen lab,

I am doing Cyb's ATB hybrid tek with Earthwalker's defat & mini-A/B for ACRB. Just finished my defat but for some reason my top non-polar layer (naphtha from first pull) is clear not brown like in Earthwalker's post? The bottom acidic aqueous layer (600 mL vinegar solution at pH 2.8 ) did turn cloudy. Not sure if this is OK? Vigorously shook it for 60 second then let sit for 5 minutes, ten times.

Could this be due to my letting the basified bark mixture cool to about room temperature before adding warm naphtha in the initial pull? EW seems to say this in his post here:

I will proceed to the mini-A/B and save the top naphtha layer just in case. Just wanted to check and see if it's something I maybe did wrong or can work to correct.

Thanks!

God morning aprobablewave , yeah sometimes the solvent gets more yellowing with the soup being warmer , so don't freak out just yet !

Endlessness - I think it did destroy the DMT with the fast-IPA-evap.

The changa seems to be harmaloid only - no dmt-effects are felt.