A fast run Down of my S to B extraction please help

[fun_guy88]

Hello every one I just want to run this down and help me answer any questions i have so here we go!

I am doing a S to B extraction so I took a LB of MHRB and crushed it up...not powder fine but still pretty good. put that in a large wine glass jug with water and one LB of LYE

then shake and letting it sit in a hot water bath for a few hours and adding VM&P the that solution shake jug and suck out the VM&P and add to a collection jug

then from there make a mixture of PH plus and water and ad that to the collection jug quickly shake and separate the two layers and do that about 3 or 4 times until most of the impurities are gone.

following that take some epson salt and cook it in the microwave for a little while take a chunk of that drop it into the new collection jug shake a little bit and then quickly separate the two layers that form.

No once the solution has been washed and dryed have it in the freezer for about 72 hours and allow to freeze into crystials

This is where I get lost....

What are the best ways to get the product out of solvent.....then also how do i go about doing a recrystallization do I then take my crystals heat up more VM&P drop the crystals in than and allow it to freeze again?

Any tips or anything would be a huge help thank you so much!

 

[57u133]

Def check the STB section, and basically all the xtract methods as most give a small rundown of re-xtal. Basically, assuming you have done things accordingly and have a decent clean product (white xtals), then you really need bestine. You can find in most art supply stores (it is rubber cement remover).
NEVER WORK AROUND OPEN FLAMES
Boil a pot of water.
Turn off.
Put in empty shot glass, so NO water gets in either.
Put in shot glass of bestine.
Let them both heat, definitely the bestine.
Put your powder in the clean shot glass.
Put hot bestine in to disovle powder.
Let get to room temperature, then put in another xtal or some more powder if no xtals yet...maybe the powder isn't as good as xtals?
The longer the better to evaporate I'm told.

5

 

[fun_guy88]

Def check the STB section, and basically all the xtract methods as most give a small rundown of re-xtal. Basically, assuming you have done things accordingly and have a decent clean product (white xtals), then you really need bestine. You can find in most art supply stores (it is rubber cement remover).
NEVER WORK AROUND OPEN FLAMES
Boil a pot of water.
Turn off.
Put in empty shot glass, so NO water gets in either.
Put in shot glass of bestine.
Let them both heat, definitely the bestine.
Put your powder in the clean shot glass.
Put hot bestine in to disovle powder.
Let get to room temperature, then put in another xtal or some more powder if no xtals yet...maybe the powder isn't as good as xtals?
The longer the better to evaporate I'm told.

5

can you elaborate on that it is getting me confused i latterly need a first grade break down im kinda slow

 

[fun_guy88]

and what is Xtals?

 

[heavenlypursuit]

SWIM thinks the epson salt to separate layers after the sodium carbonate wash is unecessary. Never had an issue with separation, even after shaking violently. Did you make sure to have the pH water above 9 or 10 in your sodium carbonate wash?
Also, you said, after it is washed and dried you put it in the freezer? Dried? Are you evaporating the solution first then putting it into the freezer?

57 wrote: Let get to room temperature, then put in another xtal or some more powder if no xtals yet...maybe the powder isn't as good as xtals?
The longer the better to evaporate I'm told.

fun guy, if you end up getting crystals and want to recrystallize read the faq. the jist of it is not really concurrent with what 57 wrote. For example, say SWIY ends up getting one gram of semi-pure product after extraction. Please note, this is one gram DRIED crystals. SWIM should then take 20-25 ml of his solvent and follow 57's directions on heating up the naptha or bestine (use bestine if you can find it, it is awesome for re-x.) Once solvent is hot enough in the shot glass, then drop in your hypothetical gram and let sit for a minute or two. Any impurities will stick to the bottom of the shot glass. Now pour off your hot heptane or naptha into your collection jar, and put in the freezer. DO NOT EVAPORATE, 20-25 ml of hot heptane will be reduced very fast, so get it in the freezer. You can also put in the fridge first for an hour or two, then into freezer, and you'll get bigger crystals. SWIM like to go right to the freezer though. I think 57 was talking about evap after you do your initial pulls, so you don't end up with too much solvent, which will in turn negatively affect your crystallization.

 

[57u133]

Heavenly,
I wasn't talking about that...but think you may have a better suggestion/more experience.
Do you always stick your hot bestine (after pouring off into collection jar) into freezer?
I thought slow evap was best...
THX

PS: Xtal=crystal

 

[fun_guy88]

Ok sounds good. Swim has some naptha in his jug separating right now...... If he sucks out as much as he can there, can he switch to BESTINE for the next 3 pulls? is that safe?

Also each pull should be in a different jar you will end up with more Xtals that way?

And awesome explanation on the recrystallization...... Just take my shot glass use a hot plate heat impurities will separate at the bottom....suck up top layer with turkey baster and put in freezer if im understanding that correctly .

 

[heavenlypursuit]

Heavenly,
I wasn't talking about that...but think you may have a better suggestion/more experience.
Do you always stick your hot bestine (after pouring off into collection jar) into freezer?
I thought slow evap was best...
THX

PS: Xtal=crystal

57,

Sorry, was not trying to say you were wrong or anything. SWIM only puts his hot heptane immediately in the freezer for recrystallization, he evaps his heptane when he is doing his initial pulls. SWIM has been told evap with heptane is not as necessary as it is with naptha, but SWIM is convinced it helps after one is done doing their pulls.

 

[heavenlypursuit]

Ok sounds good. Swim has some naptha in his jug separating right now...... If he sucks out as much as he can there, can he switch to BESTINE for the next 3 pulls? is that safe?

-----------------> Yes.

Also each pull should be in a different jar you will end up with more Xtals that way?

-----------------> Depends on how large your pulls are. SWIM only does small extractions, 50-100g, so he puts all 4 pulls into one tray, evaps off some heptane, then puts in freezer. I believe you said you were doing an extraction on a pound, so it's best to put each pull in it's own collection jar, but I like pyrex flat trays better. Much easier to get to your finished product. Remember this though. Since you are doing large pulls with naptha, make sure to evap the naptha down a bit before putting into freezer. You'll notice your solution start to get cloudy during evap, at that point put the collection jar into the freezer. If you don't see cloudiness, just evap down to about 50% of the volume of solvent used, then put in freezer. Cloudiness in the solution will ensure you have good precipitation though.

And awesome explanation on the recrystallization...... Just take my shot glass use a hot plate heat impurities will separate at the bottom....suck up top layer with turkey baster and put in freezer if im understanding that correctly .

Right on track. Most of the time you will not even have to suck up the top layer with a baster because the impurities stick pretty good to the bottom of the shot glass.
Good luck man, and report back with hopefully some success.

 

[fun_guy88]

OK guys Im at the moment of truth were im a little nervous....

I have 2 pulls so far each in different Mason jars they have been washed with PH up and Dried with Epsom salt... One pull was with Naphtha and it came out very yellow urine color like.... The other I did with Bestine and this came out almost water clear!!!! now does that sound about right?


Now I have these two jars (I dont have any pyrex dish. I have on baking dish I could use I think but it would be pretty full because the dish is small....

But n e ways what are my options use the baking dish pour one pull in it allow to sit outside in front of a box fan for a hour or so then...pop in the freezer for 72 hours followed by pulling them out finish off the evaporation and scrap off the xtals?

Or what if i decide not to go the baking dish route? what can I do with these mason jars?

 

[fun_guy88]

Also one more thing.... If I have an electric hot plate (scientific) Could I just turn that on and put a glass shot glass on top of it with the bestine in it and heat it that way?

Would the glass shatter? Also to what temperature do I want to get the bestine?

 

[heavenlypursuit]

Also one more thing.... If I have an electric hot plate (scientific) Could I just turn that on and put a glass shot glass on top of it with the bestine in it and heat it that way?

Would the glass shatter? Also to what temperature do I want to get the bestine?

If the glass is borosilicate it won't crack, not sure about shot glass, never used on electric hot plate. Just do the boil procedure first to heat up bestine. SWIM gets his to about 160-180F before he adds spice for re-x.

 

[heavenlypursuit]

OK guys Im at the moment of truth were im a little nervous....

I have 2 pulls so far each in different Mason jars they have been washed with PH up and Dried with Epsom salt... One pull was with Naphtha and it came out very yellow urine color like.... The other I did with Bestine and this came out almost water clear!!!! now does that sound about right?

---------> Still not sure what you mean by "dried with epsom salt". And as in pH up, are you talking about pH up that is used to adjust water for plants, did you wash your spice directly with that, or a water solution that was basified with sodium carbonate? Would not recommend washing directly with ph Up if thats what you did.


Now I have these two jars (I dont have any pyrex dish. I have on baking dish I could use I think but it would be pretty full because the dish is small....

But n e ways what are my options use the baking dish pour one pull in it allow to sit outside in front of a box fan for a hour or so then...pop in the freezer for 72 hours followed by pulling them out finish off the evaporation and scrap off the xtals?

----------> Pretty much. After each pull, evaporate that pull down until it gets cloudy or a good portion of the solvent has been evaped off. Try and fit one pull in your baking dish and you will see how much easier it is to get to your product when its ready, it shouldn't be a problem after you evap some off anyways. After letting it sit in the freezer for your desired time, pour or decant off your solvent from the spice, flip the jar or tray upside down in the freezer for an hour or two to get any remaining solvent out of the spice, then take out of the freezer and put in front of a fan for an hour or so to evap the last trace amounts of naptha/bestine. Scrape up and enjoy, or re-x, then enjoy. SWIM thinks at least one re-x is necessary, he does three.

Or what if i decide not to go the baking dish route? what can I do with these mason jars?

 

[57u133]

thx Heavenly
Didn't think you were disclaiming what I was suggesting, but I am always looking for better methods...I never mind if someone tells SWIM they were wrong...especially if helps.

 

[fraterS.O.L.]

Slow evaporating does make WAY bigger xtals. Do just as heavenly said but after you pour of your 20-25ml into another (double) shot glass put in another 25-30ml bestine. put some plastic wrap on top and poke a hole in it so it slows the evap down and sit it in a cool dark place and DON'T touch it for a day or two. This shoul give you some big shards but the excess solvent and minimal air flow is key to getting it to evap as SLOOOOW as possible

 

[57u133]

frater,
This extra solvent idea is interesting. Do you know why reaction-wise more solvent, after the first bestine 'pull' into a clean shot glass, works well?

I just realized the times I had bigger crystals I used more solvent than recommended...

 

[fraterS.O.L.]

I'm no chemist but I believe its just to slow the evaporation down. Think, 25ml of HOT heptane will evap real quick, however if you add another 25ml of heptane that hasnt been heated it helps cool the solution a tad and gives more room for the molecules to move. Restricting the airflow e.g. plastic wrap with the hole in it will increase the time of the evap even more. Basically, the SLOWER the solution evaporates the BIGGER the xtals grow. Not 100% on why, but 100% sure it works.

 

[57u133]

Started a new batch with the information given. Results posted soon.

 

[endlessness]

To the OP, always check the FAQ before asking questions, as many of your questions may be answered there.. For example:

FAQ: Whats the best way to retrieve crystals after freezing

and


FAQ: How does one recrystallize

If you are wondering what is best, evaporating or freezing for the first retrieval, well, it depends, theres advantages and disadvantages. Freezing will usually yield cleaner product and you can reuse the naphtha after freezing. Evaporating is better for those that dont have a freezer or cant use it for these purpouses or if they want to leave it evaporating for very long for growing large crystals.



As for the 'why do crystals grow larger with more solvent/slower evap/freeze', crystals tend to form together, but if you do it fast, they are 'forced' to precipitate in small chunks. If you evap slower, they will be able to form on top of each other. Also movement (air movement or whatever) will disturb larger crystal formation. So the slower evap (closing the container and leaving very small opening to evap, and/or putting in a place with little air movement and not warm), the bigger the crystals grow. If you have just enough solvent for the dmt, it will start precipitating right as it cools down and/or evaporates a bit, so they wont grow so big. On the other hand if you have more solvent there is larger time for it to slowly start precipitating, so it grows larger crystals. But if you are recrystallizing, you need to use only a small amount of solvent as explained on link above, otherwise you will pull all impurities together so it wont make any difference to the product purity. What you could do is use the right amount of solvent to recrystallize, and then after separating the solvent from the bottom goo, adding more solvent to it and evaporating it slowly. You cant really add more solvent and then freeze because for freezing you want the least amount of solvent per dmt as possible otherwise it wont be saturated enough and some might not precipitate.

Also another way to grow crystals appart from slow evap is the container between freezer and fridge will grow larger crystals every couple of hours over a few days, because as you move from freezer into fridge and it warms up, the smaller crystals will dissolve first, and once you move back into the freezer, the crystals will tend to form on top of the bigger crystals that are already formed.

Do note, though, that crystal growing has no real practical use, wont make the trip better or something, but it is very nice just for the sake of it, like an alchemical experience

 

[fun_guy88]

OMG I need help

So I had my mason jars with 400 ml of liquid each in them left in the freezer for about 3 or 4 days after that I opened them up and dumped it out into a baking dish and put a fan in front of it.... Now all im left with is yellow goo that looks and smells like spice but its not turning crystals or powder its just staying goo like. its been in front of the fan for about 8 hours now do you think it just needs more time?