Righty-o good sir, will do.

Hey sorry guys - This is a beginner question but I have been using the search function for the past 15 mins or so and can't find an answer. I am having a hard time pulling pure limonene off of the top of my MHRB mixture using the BLAB tek. A few drops of the dark MHRB always make their way into the limonene when I try to pull it. Is this acceptable? I am working with a syringe, but I also have a gravy separator. I would be using the separator but I'm not really sure how to go about it. I added approx 50ml of additional water to it already as advised in a different thread; it helped but still having trouble.
Are there any tips or tricks for getting a clean layer of limonene off the top?

EDIT - Ahh nevermind, wasn't looking hard enough evidently - Found what I was looking for. Thanks!

I keep getting Yellow wax, Green Wax, or Nothing at all on evaps, and on freezing I get Ice crystals, which sometimes dry to leave a bit of NaOH but no spice, not even a sniff. This happens even when I evap off most of the shell before the freeze. Now up to 20+ attempts, have tried all sorts of Acacia, including Obtusifolia and Longfolia - both leaf and bark, as well as polyrodifolia, and a couple of other Acacias (just for luck). I am using Mechanix caustic, and Diggers Shellite, and grind the material up to a fine powder. Yes the shell is nice and hot and I have been using a pH meter (broken now...). I am now following a version of Lextek, but I am doing a double acid base, after being shown this method by a mate who can cook spice. I get no pretty spice smell - EVER - and when I try smoking the wax stuff, it just shuts down the lungs - with no spice effect at all. When I try to filter the crystals, they always melt and dissappear. I have tried re-crystalising the wax - but I just get more wax. The wax also dissolves completely in alcohol, and evaps back to ..... Wax!. Left to sit, it never dries (weeks...) When I do dry out the jar after a freeze , sometimes I get a bit of white powder that seems to be just NaOH. I have tried filtering the shell, and doing Na Carbonate washes, and being really pedantic to get the water out before freezing - but Nada - no spice. It is really frustrating as having had a taste of the real spice (via mate), I want to go back there again. If I hadn't tried it, I would now believe that this whole thing is an internet hoax, but instead, I am just getting annoyed and wasting a lot of money making very small ammounts of water ice. I suspected nasties in my solvents etc - but having read the forums here - I note others seem to be suceeding with the same stuff I am using. Don't know how to get MHRB in Melbourne, don't think it is safe to order online in Oz, and havent got a lot of $$$$ to throw around. Am I cursed by the spice gods??? Can anyone offer a clue - coz I don't seem to have one - neither does my mate who lives interstate, and gets a different Acacia to the ones I have access to.

are you using naphtha or other solvents? couse some solvents doesn't freeze precipit out the goods..

I am using Diggers Shellite, it's a different brand to what works for mate, but no other type available at shops near me and I am pretty sure others on the nexus have reported sucess with this solvent. I am starting to get very sus of the other 2% in my 98% pure NaOH. I am thinking of exploring other solvents, but not sure which one to try first - they all seem harder to work with than shellite for freeze precep (according to reports).

i don't think it could be a problem of your lye..but if theese 2% are maybe emulsifier so it could be a problem..

Thanks everyone for the advice, I appreciate it, and will post the answer to this problem when I figure it out.
(To save the next poor shmuck from 21+ failed attempts)

Emulsifier in the 2% would make sense, as when my mate tried to extract using my caustic and some plant material that he knew was good, the layers did not separate like normal. I haven't been having trouble getting layers to separate myself. I will be trying a few other solvents aside from shellite, as I am so sick of spice-less jars coming out of the freezer!!! I am also now trying to make my own NaOH - by electrolysis - to make sure it is relatively pure of nasty contaminants.

Spice - one taste and the world never quite seems the same again!

very sad hearing about doing your own lye by electrolisis

Hello, a man in my imagination will begin an extraction within the next few days following Q21Q21's second tek. He was the one who was going to rush this for new years but circumstances changed and he will be doing it now instead. He was going to perform a side-by-side test with the same bark to test for n-oxide but circumstances may be against this happening, unless he can figure out an easy way to substitute naptha in the non-polar wash of the tek to pull out n-oxide dmt. He will keep his updates here if that's cool.

Re making NaOH via electrolysis - yeah, not so keen to do it either, read about the chlorine gas it evolves and it seems a lot of hassle , likely to contain impurities. Very open to other ideas / suggestions - SWIM checked online, however it seems getting pure NaOH is becoming difficult, Haven't been able to find pure NaOH on the shelf at local shops, many online local places either don't sell it or don't ship, also SWIM doesn't want to start ordering chemicals online from overseas...;-} SWIM will be trying the local soap making supply shop soon, and thinks making home made soap might be fun, too!

Good news is SWIM now has some other solvents, and will be giving some other teks a go, including the D limonlene organic and Toluene jungle spice.

SWIM also intends to double check the species identification, and maybe explore another species, such as Desmodium.
SWIM has had so much practice now, he is proficient in the chem, and so less certain that the organic material is good.

We shall not be defeated.......!!!!

If you can get fumaric acid, salt the limonene with FASI or FASW and do the slow water crystallization as in BLAB. Good luck!

Hey guys - I have been following the BLAB to a tee but unfortunately got some brownish/red goo precipitating on the bottom of my FASI/Limo mix. To fix this I followed the BLAB and added 20ml water, mixed it, and then evaporated it. Now I have this after roughly 15 mins of evapping:


Very thick goo that I imagine will dry into a hard sheet. This is similar to what someone in the BLAB thread posted but I am unclear on what to do with it. I know you cannot tell much on sight alone, but does it look alright?

So after this sheet hardens, do I just break it up and scrape it off and that is my fumarate?

Sorry for the noob question, this is my first time. I'm going to run through this thread and see if this question has already been addressed as well. I've read a bit about the "yellow goo" which I think is what I have? But I wasn't using Naptha so I don't know if the rules change?

Dont evaporate it in a metal container for starters, are you gonna start scrapping the metal together after its finished? I suggest you add a bit of hot water and let it evaporate in a glass container... scrape it up/let it dry as much as possible, hopefully it hardens up. If it never does harden up after spreading it around and letting it air dry for long, recrystallize it with acetone or IPA (just redissolve in minimal amount of hot IPA/acetone and stick in the freezer for a couple of days)

remember dont throw anything away until its all finished, your alkaloids are never lost if you dont discard things.

First off - Thanks man, I've been reading your posts throughout this thread and they've all been really helpful.

That stove only works with steel containers or I would've used glass. I scraped off the hardened layer and it actually turned out looking pretty good. The parts of the layer I couldn't get off I dissolved in warm water like you said and put that into a glass container to evaporate in my oven (should've used the oven in the first place).

Thanks again dude, my yield wasn't good, but I am just glad to have something to show for my work.

Glad to be of help

How comes the yield wasnt good? Are you finished with the extraction or still doing more pulls? If bark is good, you can likely just keep pulling and more will come off.. Also if you didnt add enough FASI to limo, maybe not all the alks crashed out of limo....

You can recrystallize that fumarate if you want.. I suggest you trying out recrystallization with half of the product, see what comes out, compare both and see if its worth it to recrystallize, how much yield is lost, how cleaner it looks, etc... Again, just remember not throw anything out (for example the acetone/IPA after freezing), because if yield is somehow bad you can always retrieve your stuff back

That was the culmination all my pulls, but with your advice I think I'll try for more - it is sometimes easy for me to forget that the good stuff is in there, it is just a matter of getting it out. I'll do a re-crystallization with a sample of what I've got and let you know how it goes.

I'm guessing you're familiar enough with the chemistry of the extraction that you don't follow a specific tek?

OK SWIM has got some powdered mhrb and tried their first extraction ... not going well so far:

Any help would be greatly appreciated by SWIM.

Using Lazy man's guide at half measures (no defat)
250G MHRB
100g NaOH
1l water
Mixed and set aside for a few hours - BLACK and THICK
Added 125ml Naptha (Zippo Fuel)
Electric beater on low for 5 minutes (here was my mistake )
No layer and REAL thick so SWIM added another 500ml Basified water (50g NaOH)
Added another 125ml of Naptha - Stirring this time - no more vigorous mixing!!!!!!!
SWIM was able to pull off about 50ml of naptha off the top and evaporated this to a lump of orange goo about 3 rice grains big after scraping up.
SWIM said this smelt right so tried to smoke it ... SWIM says that it went very, very well but did feel a bit nauseous afterward.
SWIM now has pot in warm water trying to get separation and has got another 30ml but it is very orange:


SWIM is wondering if there's another way to get better separation with current batch?
Is the Freezing method better to get crystals?
Anything else?

Thanks
Craig

OK so SWIM continued and tried:
15g NaCl in a hot bath .... no difference
200ml warm Shellite stir - got 130ml pull evap'd to 35ml and freeze precip (brown stuff in the bottom of jar)
Test PH 12.2 => added 75g NaOH to 750ml water and added to mix
PH 13.5
200ml Cold shellite stirred 15mins ... evap'd to 25% and Freeze precip (brown again)
500ml warm Shellite, stirred 5 mins, pulled 460ml dark orange, evap'd to 25% and FP (See Picture)
500ml cold shellite, stirred 5 mins, pulled 400ml of near colourless. completely evap'd to oily creamy stuff that didn't smell right.
Will Re-Basify and SWIM try again on monday .....

Is this brown stuff that SWIm's looking for? Doesn't look very crystaline. If SWIM gets some out and get it to room temp it melts to oily sludge that doesn't smell right. SWIM said that his mix still smells more like DMT that this sludge.

SWIM is wondering what he's doing wrong?

I think you're pulling some of the basified liquid together, maybe its suspended in very small droplets that you dont notice and once its frozen it accumulates in one part and forms this sludge. That could have to do with prepowdered bark+mixing/shaking too strongly, hard to say.

In any case try doing a sodium carbonate wash before freezing. Otherwise you should make several pulls (or put together the stuff you already pulled), combine them, then salt them out with vinegar 2 or 3x, discard the solvent, basify that vinegar and extract the basified vinegar with fresh solvent, and then into the freezer

good luck